Ethanol hydrochloride → HCID 70109635, compound

HRID 356150Notes

Reaction equation

HRID 356150 reaction equation
Cl.C(O)C.[Cl:5][C:6]1[CH:27]=[C:26]([Cl:28])[CH:25]=[CH:24][C:7]=1[CH2:8][N:9]1[C:15](=[O:16])[C@H:14]2[CH2:17][CH2:18][CH2:19][C@H:13]2[NH:12][C:11]2[CH:20]=[CH:21][CH:22]=[CH:23][C:10]1=2>C(OCC)C>[ClH:5].[Cl:5][C:6]1[CH:27]=[C:26]([Cl:28])[CH:25]=[CH:24][C:7]=1[CH2:8][N:9]1[C:15](=[O:16])[C@H:14]2[CH2:17][CH2:18][CH2:19][C@H:13]2[NH:12][C:11]2[CH:20]=[CH:21][CH:22]=[CH:23][C:10]1=2

Participants

4

Reactant 2

HCID 21887872Ethanol hydrochlorideHCID 70109636HCID 70109636, compound

Product 1

HCID 70109635HCID 70109635, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

In diethylether was dissolved (3aR*,10aS*)-9-(2,4-dichlorobenzyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one produced in Working Example 22. To the solution was added a 2.5N hydrogen chloride-ethanol solution, and the mixture was stirred. Resulting crystalline precipitate was collected by filtration to obtain the titled compound, m.p. 164°-167° C.

Workup

  1. customproduced in Working Example 22
  2. filtrationResulting crystalline precipitate was collected by filtration

Sources & evidence

ORD record
ord-90e8fdbbc3f744b88ea519da798a7ae5
Source dataset
uspto-grants-1998_11
Patent number
US05834463

Reaction notes

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