Hydrazine hydrate (1:1) → HCID 178514332, compound

HRID 2082442Notes

Reaction equation

HRID 2082442 reaction equation
[Br:1][C:2]1[CH:19]=[CH:18][C:5]2[N:6]3[CH2:17][CH2:16][C:15]4[C:7]3=[C:8]([CH:12]=[CH:13][CH:14]=4)[C:9](=S)[NH:10][C:4]=2[CH:3]=1.O.[NH2:21][NH2:22]>C1C=CC=CC=1>[Br:1][C:2]1[CH:19]=[CH:18][C:5]2[N:6]3[CH2:17][CH2:16][C:15]4[C:7]3=[C:8]([CH:12]=[CH:13][CH:14]=4)[C:9](=[N:21][NH2:22])[NH:10][C:4]=2[CH:3]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 15132540HCID 15132540, compound

Product 1

HCID 178514332HCID 178514332, compoundYield 59.5%

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

9-Bromo-1,2-dihydrobenzo[b]pyrrolo[3,2,1-jk][1,4]benzodiazepin-6-thione (4 g), hydrazine hydrate (4 ml) and benzene (150 ml) were combined and refluxed overnight. The reaction mixture was concentrated to approximately 50 ml and, after standing overnight, the precipitate was filtered. Recrystallization of the filter cake from chloroform/ether gave 2.35 g (59.5%) of product, mp 260° C. (dec).

Workup

  1. temperaturerefluxed overnight
  2. concentrationThe reaction mixture was concentrated to approximately 50 ml
  3. filtrationthe precipitate was filtered
  4. customRecrystallization of the filter cake from chloroform/ether

Sources & evidence

ORD record
ord-6f1bf1b1ce674c53829263872ec45ad6
Source dataset
uspto-grants-1993_02
Patent number
US05189161

Reaction notes

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