Water → HCID 12434308, compound

HRID 262972Notes

Reaction equation

HRID 262972 reaction equation
[C:1]1([C:7]2[C:8]3[CH:17]=[CH:16][S:15][C:9]=3[NH:10][C:11](=S)[CH2:12][N:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:18]([NH:21][NH2:22])(=[O:20])[CH3:19].O>C(O)C>[C:18]([NH:21][NH:22][C:11]1[CH2:12][N:13]=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:8]2[CH:17]=[CH:16][S:15][C:9]=2[N:10]=1)(=[O:20])[CH3:19]

Participants

5

Reactant 3

HCID 962WaterHCID 14039AcetohydrazideHCID 135848425HCID 135848425, compound

Product 1

HCID 12434308HCID 12434308, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

1.5 g (0.00582 mol) of 1,3-dihydro-5-phenyl-2H-thieno[2,3-e]-1,4-diazepine-2-thione are heated to reflux for 4 hours under a nitrogen atmosphere with 1.3 g (0.0175 mol) of acetyl hydrazine in 120 ml of absolute ethanol. The solvent is evaporated and the crystals obtained are shaken with water in a separating funnel. After filtration under a vacuum, the product is recrystallized from ethyl acetate containing active carbon to give colorless crystals of 2-(2-acetylhydrazino)-5-phenyl-3H-thieno[2,3-e]-1,4-diazepine, melting point 194°-196° C. (transition).

Workup

  1. customThe solvent is evaporated
  2. customthe crystals obtained
  3. filtrationAfter filtration under a vacuum
  4. customthe product is recrystallized from ethyl acetate containing active carbon

Sources & evidence

ORD record
ord-bc8f5b758ef74f78b82c2e411193a74f
Source dataset
uspto-grants-1979_05
Patent number
US04155913

Reaction notes

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