HCID 21317692, compound → Fluclotizolam

HRID 262976Notes

Reaction equation

HRID 262976 reaction equation
[C:1]([NH:4][NH:5][C:6]1[CH2:7][N:8]=[C:9]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[F:23])[C:10]2[CH:15]=[C:14]([Cl:16])[S:13][C:11]=2[N:12]=1)(=O)[CH3:2]>C1(C)C(C)=CC=CC=1>[Cl:16][C:14]1[S:13][C:11]2[N:12]3[C:1]([CH3:2])=[N:4][N:5]=[C:6]3[CH2:7][N:8]=[C:9]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[F:23])[C:10]=2[CH:15]=1

Participants

3

Reactant 1

HCID 21317692HCID 21317692, compound

Product 1

HCID 21317700Fluclotizolam

Reagents, catalysts & solvents 1

HCID 7237O-XyleneSolvent

Procedure

6.8 g of 2-(2-acetylhydrazino)-7-chloro-5-(o-fluorophenyl)-3H-thieno[2,3-e]-1,4-diazepine are refluxed for 9 hours in 300 ml of absolute xylene. After cooling, the precipitated impurities are filtered off under vacuum. The solvent is then evaporated under reduced pressure and the product recrystallized from ethyl acetate containing active carbon to yield 2-chloro-4-(o-fluorophenyl)-9-methyl-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine, melting point 187°-189° C.

Workup

  1. temperatureAfter cooling
  2. filtrationthe precipitated impurities are filtered off under vacuum
  3. customThe solvent is then evaporated under reduced pressure
  4. customthe product recrystallized from ethyl acetate containing active carbon

Sources & evidence

ORD record
ord-705bf0a3a623430d9df117106fb0cbe8
Source dataset
uspto-grants-1979_05
Patent number
US04155913

Reaction notes

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