1,4-Dimethylpiperazine
货号 B091421
:
106-58-1
分子量: 114.19 g/mol
InChI 键: RXYPXQSKLGGKOL-UHFFFAOYSA-N
注意: 仅供研究使用。不适用于人类或兽医用途。
Patent
US09115160B2
Procedure details
Bis(2-chloroethyl)amine hydrochloride (5 g, 0.028 mol) is put into a 100 mL two-necked flask, and N,N′-Dimethylpiperazine (7.1 eq) is added into the flask. After cooling the flask and the reactants therein to about 4° C., POCl3 (4.49 g, 1.04 eq) is slowly dropped into the flask, and the mixture in the flask is stirred at room temperature for 5 hours. After that, the mixture in the flask is cooled to about 4° C., and 3-aminopropanol (2.1 g, 1.0 eq) is slowly dropped into the flask for 3 hours. After adding 3-aminopropanol into the flask, the mixture in the flask is stirred at room temperature for 15 hours. (The conversion yield determined with HPLC is about 11.84%.)
Name
Identifiers
|
REACTION_CXSMILES
|
Cl.[Cl:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][Cl:8].CN1CCN(C)CC1.[O:17]=[P:18](Cl)(Cl)Cl.[NH2:22][CH2:23][CH2:24][CH2:25][OH:26]>>[CH2:24]1[CH2:25][O:26][P:18]([N:5]([CH2:6][CH2:7][Cl:8])[CH2:4][CH2:3][Cl:2])(=[O:17])[NH:22][CH2:23]1 |f:0.1|
|
Inputs
Step One
|
Name
|
|
|
Quantity
|
5 g
|
|
Type
|
reactant
|
|
Smiles
|
Cl.ClCCNCCCl
|
Step Two
|
Name
|
|
|
Quantity
|
0 (± 1) mol
|
|
Type
|
reactant
|
|
Smiles
|
CN1CCN(CC1)C
|
Step Three
|
Name
|
|
|
Quantity
|
4.49 g
|
|
Type
|
reactant
|
|
Smiles
|
O=P(Cl)(Cl)Cl
|
Step Four
|
Name
|
|
|
Quantity
|
2.1 g
|
|
Type
|
reactant
|
|
Smiles
|
NCCCO
|
Step Five
|
Name
|
|
|
Quantity
|
0 (± 1) mol
|
|
Type
|
reactant
|
|
Smiles
|
NCCCO
|
Conditions
Temperature
|
Control Type
|
AMBIENT
|
Stirring
|
Type
|
CUSTOM
|
|
Details
|
the mixture in the flask is stirred at room temperature for 5 hours
|
|
Rate
|
UNSPECIFIED
|
|
RPM
|
0
|
Other
|
Conditions are dynamic
|
1
|
|
Details
|
See reaction.notes.procedure_details.
|
Workups
TEMPERATURE
|
Type
|
TEMPERATURE
|
|
Details
|
After cooling the flask
|
TEMPERATURE
|
Type
|
TEMPERATURE
|
|
Details
|
After that, the mixture in the flask is cooled to about 4° C.
|
STIRRING
|
Type
|
STIRRING
|
|
Details
|
the mixture in the flask is stirred at room temperature for 15 hours
|
|
Duration
|
15 h
|
CUSTOM
|
Type
|
CUSTOM
|
|
Details
|
(The conversion yield
|
Outcomes
Product
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. |
