Pyridoxine-d5
Cat. No. B025862
M. Wt: 174.21 g/mol
InChI Key: LXNHXLLTXMVWPM-WNWXXORZSA-N
Attention: For research use only. Not for human or veterinary use.
Patent
US07214799B2
Procedure details
In a second alternative and preferred workup, the reaction mixture (following complete conversion to compound (C)) is cooled to 20° C. and diluted with water (approximately 2.80 L of water for every 1 kg of starting pyridoxine HCl). After phase separation the organic phase is washed with water. The combined aqueous phases are reextracted twice with TBME. The combined TBME phases are washed once with saturated NaHCO3-solution and once with diluted brine. The MTBE-product solution is concentrated to a concentration of about 50% and stored at room temperature until it is further converted. If this second alternative workup is used, the volume of MTBE in the synthetic step is preferably reduced by about 26%.
[Compound]
Name
compound ( C )
Quantity
0 (± 1) mol
Type
reactant
Reaction Step One
Identifiers
|
REACTION_CXSMILES
|
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([CH2:10][OH:11])[C:3]=1[OH:12].Cl>O>[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([CH2:10][OH:11])[C:3]=1[OH:12] |f:0.1|
|
Inputs
Step One
[Compound]
|
Name
|
compound ( C )
|
|
Quantity
|
0 (± 1) mol
|
|
Type
|
reactant
|
|
Smiles
|
|
Step Two
|
Name
|
|
|
Quantity
|
1 kg
|
|
Type
|
reactant
|
|
Smiles
|
CC1=C(C(=C(C=N1)CO)CO)O.Cl
|
|
Name
|
|
|
Quantity
|
0 (± 1) mol
|
|
Type
|
solvent
|
|
Smiles
|
O
|
|
Name
|
|
|
Quantity
|
2.8 L
|
|
Type
|
solvent
|
|
Smiles
|
O
|
Conditions
Other
|
Conditions are dynamic
|
1
|
|
Details
|
See reaction.notes.procedure_details.
|
Workups
CUSTOM
|
Type
|
CUSTOM
|
|
Details
|
After phase separation the organic phase
|
WASH
|
Type
|
WASH
|
|
Details
|
is washed with water
|
WASH
|
Type
|
WASH
|
|
Details
|
The combined TBME phases are washed once with saturated NaHCO3-solution and once with diluted brine
|
CONCENTRATION
|
Type
|
CONCENTRATION
|
|
Details
|
The MTBE-product solution is concentrated to a concentration of about 50%
|
CUSTOM
|
Type
|
CUSTOM
|
|
Details
|
stored at room temperature until it
|
Outcomes
Product
|
Name
|
|
|
Type
|
|
|
Smiles
|
CC1=C(C(=C(C=N1)CO)CO)O
|
Source
|
Source
|
Open Reaction Database (ORD) |
|
Description
|
The Open Reaction Database (ORD) is an open-access schema and infrastructure for structuring and sharing organic reaction data, including a centralized data repository. The ORD schema supports conventional and emerging technologies, from benchtop reactions to automated high-throughput experiments and flow chemistry. Our vision is that a consistent data representation and infrastructure to support data sharing will enable downstream applications that will greatly improve the state of the art with respect to computer-aided synthesis planning, reaction prediction, and other predictive chemistry tasks. |
Patent
US07214799B2
Procedure details
In a second alternative and preferred workup, the reaction mixture (following complete conversion to compound (C)) is cooled to 20° C. and diluted with water (approximately 2.80 L of water for every 1 kg of starting pyridoxine HCl). After phase separation the organic phase is washed with water. The combined aqueous phases are reextracted twice with TBME. The combined TBME phases are washed once with saturated NaHCO3-solution and once with diluted brine. The MTBE-product solution is concentrated to a concentration of about 50% and stored at room temperature until it is further converted. If this second alternative workup is used, the volume of MTBE in the synthetic step is preferably reduced by about 26%.
[Compound]
Name
compound ( C )
Quantity
0 (± 1) mol
Type
reactant
Reaction Step One
Identifiers
|
REACTION_CXSMILES
|
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([CH2:10][OH:11])[C:3]=1[OH:12].Cl>O>[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([CH2:10][OH:11])[C:3]=1[OH:12] |f:0.1|
|
Inputs
Step One
[Compound]
|
Name
|
compound ( C )
|
|
Quantity
|
0 (± 1) mol
|
|
Type
|
reactant
|
|
Smiles
|
|
Step Two
|
Name
|
|
|
Quantity
|
1 kg
|
|
Type
|
reactant
|
|
Smiles
|
CC1=C(C(=C(C=N1)CO)CO)O.Cl
|
|
Name
|
|
|
Quantity
|
0 (± 1) mol
|
|
Type
|
solvent
|
|
Smiles
|
O
|
|
Name
|
|
|
Quantity
|
2.8 L
|
|
Type
|
solvent
|
|
Smiles
|
O
|
Conditions
Other
|
Conditions are dynamic
|
1
|
|
Details
|
See reaction.notes.procedure_details.
|
Workups
CUSTOM
|
Type
|
CUSTOM
|
|
Details
|
After phase separation the organic phase
|
WASH
|
Type
|
WASH
|
|
Details
|
is washed with water
|
WASH
|
Type
|
WASH
|
|
Details
|
The combined TBME phases are washed once with saturated NaHCO3-solution and once with diluted brine
|
CONCENTRATION
|
Type
|
CONCENTRATION
|
|
Details
|
The MTBE-product solution is concentrated to a concentration of about 50%
|
CUSTOM
|
Type
|
CUSTOM
|
|
Details
|
stored at room temperature until it
|
Outcomes
Product
|
Name
|
|
|
Type
|
|
|
Smiles
|
CC1=C(C(=C(C=N1)CO)CO)O
|
Source
|
Source
|
Open Reaction Database (ORD) |
|
Description
|
The Open Reaction Database (ORD) is an open-access schema and infrastructure for structuring and sharing organic reaction data, including a centralized data repository. The ORD schema supports conventional and emerging technologies, from benchtop reactions to automated high-throughput experiments and flow chemistry. Our vision is that a consistent data representation and infrastructure to support data sharing will enable downstream applications that will greatly improve the state of the art with respect to computer-aided synthesis planning, reaction prediction, and other predictive chemistry tasks. |
Patent
US07214799B2
Procedure details
In a second alternative and preferred workup, the reaction mixture (following complete conversion to compound (C)) is cooled to 20° C. and diluted with water (approximately 2.80 L of water for every 1 kg of starting pyridoxine HCl). After phase separation the organic phase is washed with water. The combined aqueous phases are reextracted twice with TBME. The combined TBME phases are washed once with saturated NaHCO3-solution and once with diluted brine. The MTBE-product solution is concentrated to a concentration of about 50% and stored at room temperature until it is further converted. If this second alternative workup is used, the volume of MTBE in the synthetic step is preferably reduced by about 26%.
[Compound]
Name
compound ( C )
Quantity
0 (± 1) mol
Type
reactant
Reaction Step One
Identifiers
|
REACTION_CXSMILES
|
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([CH2:10][OH:11])[C:3]=1[OH:12].Cl>O>[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([CH2:10][OH:11])[C:3]=1[OH:12] |f:0.1|
|
Inputs
Step One
[Compound]
|
Name
|
compound ( C )
|
|
Quantity
|
0 (± 1) mol
|
|
Type
|
reactant
|
|
Smiles
|
|
Step Two
|
Name
|
|
|
Quantity
|
1 kg
|
|
Type
|
reactant
|
|
Smiles
|
CC1=C(C(=C(C=N1)CO)CO)O.Cl
|
|
Name
|
|
|
Quantity
|
0 (± 1) mol
|
|
Type
|
solvent
|
|
Smiles
|
O
|
|
Name
|
|
|
Quantity
|
2.8 L
|
|
Type
|
solvent
|
|
Smiles
|
O
|
Conditions
Other
|
Conditions are dynamic
|
1
|
|
Details
|
See reaction.notes.procedure_details.
|
Workups
CUSTOM
|
Type
|
CUSTOM
|
|
Details
|
After phase separation the organic phase
|
WASH
|
Type
|
WASH
|
|
Details
|
is washed with water
|
WASH
|
Type
|
WASH
|
|
Details
|
The combined TBME phases are washed once with saturated NaHCO3-solution and once with diluted brine
|
CONCENTRATION
|
Type
|
CONCENTRATION
|
|
Details
|
The MTBE-product solution is concentrated to a concentration of about 50%
|
CUSTOM
|
Type
|
CUSTOM
|
|
Details
|
stored at room temperature until it
|
Outcomes
Product
|
Name
|
|
|
Type
|
|
|
Smiles
|
CC1=C(C(=C(C=N1)CO)CO)O
|
Source
|
Source
|
Open Reaction Database (ORD) |
|
Description
|
The Open Reaction Database (ORD) is an open-access schema and infrastructure for structuring and sharing organic reaction data, including a centralized data repository. The ORD schema supports conventional and emerging technologies, from benchtop reactions to automated high-throughput experiments and flow chemistry. Our vision is that a consistent data representation and infrastructure to support data sharing will enable downstream applications that will greatly improve the state of the art with respect to computer-aided synthesis planning, reaction prediction, and other predictive chemistry tasks. |
