Water → HCID 70573353, compound

HRID 1758922Notes

Reaction equation

HRID 1758922 reaction equation
C(Cl)(Cl)[Cl:2].Cl.Cl.[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[N:17]3[CH2:18][CH2:19][N:20]([CH2:22][CH2:23]Cl)[CH2:21][CH:16]3[CH2:15][N:14]=[C:13]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:12]=2[CH:31]=1.[OH2:32]>C(O)(C)C>[ClH:2].[ClH:7].[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[N:17]3[CH2:18][CH2:19][N:20]([CH2:22][CH2:23][OH:32])[CH2:21][CH:16]3[CH2:15][N:14]=[C:13]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:12]=2[CH:31]=1

Participants

5

Reactant 3

HCID 962WaterHCID 6212ChloroformHCID 131712764HCID 131712764, compound

Product 1

HCID 70573353HCID 70573353, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent2×

Procedure

2.5 mole H2O are heated under reflux with 15 ml thionylchloride for 20 minutes. The solvent is subsequently removed and the base yielded with dilute water sodium hydroxide solution under cooling with ice and subsequently isolated from chloroform. 3.2 g of 1,2,3,4,4a,5-hexahydro-9-chloro-3-(β-chlorethyl)7-phenyl-pyrazino[1,2-a][1,4]benzodiazepinedihydrochloride.1.0 mole H2O.0.6 mole Isopropanol has been crystallized from isopropanol said compound having a freezing point of 220° C. (decomposing).

Workup

  1. temperatureunder cooling with ice

Sources & evidence

ORD record
ord-7b05c5a8f7854fb89053d25ee2081bdc
Source dataset
uspto-grants-1982_07
Patent number
US04338314

Reaction notes

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