Ethanol hydrochloride → (3aR*,10aS*)-9-(4-Nitrobenzyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one hydrochloride

HRID 356152Notes

Reaction equation

HRID 356152 reaction equation
[N+:1]([C:4]1[CH:25]=[CH:24][C:7]([CH2:8][N:9]2[C:15](=[O:16])[C@H:14]3[CH2:17][CH2:18][CH2:19][C@H:13]3[NH:12][C:11]3[CH:20]=[CH:21][CH:22]=[CH:23][C:10]2=3)=[CH:6][CH:5]=1)([O-:3])=[O:2].[ClH:26].C(O)C>C(O)C>[ClH:26].[N+:1]([C:4]1[CH:25]=[CH:24][C:7]([CH2:8][N:9]2[C:15](=[O:16])[C@H:14]3[CH2:17][CH2:18][CH2:19][C@H:13]3[NH:12][C:11]3[CH:20]=[CH:21][CH:22]=[CH:23][C:10]2=3)=[CH:6][CH:5]=1)([O-:3])=[O:2]

Participants

4

Reactant 2

HCID 21887872Ethanol hydrochlorideHCID 54563031(3aR*,10aS*)-9-(4-Nitrobenzyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one

Product 1

HCID 70111281(3aR*,10aS*)-9-(4-Nitrobenzyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one hydrochloride

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

In ethanol was suspended (3aR*,10aS*)-9-(4-Nitrobenzyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]-diazepin-10(1H)-one produced in Working Example 26. To the suspension was added an HCl-ethanol solution, and the mixture was stirred. Resulting crystalline precipitate was collected by filtration, which was washed with ethanol to give the titled compound, m.p. 167°-170° C.

Workup

  1. customproduced in Working Example 26
  2. filtrationResulting crystalline precipitate was collected by filtration, which
  3. washwas washed with ethanol

Sources & evidence

ORD record
ord-87981e42470b434ab0f2ecf55c5d4f3e
Source dataset
uspto-grants-1998_11
Patent number
US05834463

Reaction notes

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