Methylhydrazine → HCID 19699120, compound

HRID 863025Notes

Reaction equation

HRID 863025 reaction equation
[Cl:1][C:2]1[S:11][C:10]2[C:9](=O)[C:8](=[CH:13][N:14](C)[CH3:15])[CH2:7][CH2:6][N:5]([C:17](=O)[C:18]3[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=3)[C:4]=2[CH:3]=1.C[NH:29]N>CO>[Cl:1][C:2]1[S:11][C:10]2[C:9]3=[N:29][N:14]([CH3:15])[CH:13]=[C:8]3[CH2:7][CH2:6][N:5]([CH2:17][C:18]3[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=3)[C:4]=2[CH:3]=1

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 54376584HCID 54376584, compound

Product 1

HCID 19699120HCID 19699120, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
80 °C

Procedure

A mixture of 500 mg of 2-chloro-7-[(dimethylamino)methylene]-4,5,6,7-tetrahydro-4-(4-nitrobenzoyl)-8H-thieno[3,2-b]azepin-8-one in 15 ml of absolute methanol is stirred under argon while 131 μl of N-methylhydrazine is added. The reaction mixture is heated at 80° C. for 18 hours. The reaction mixture is cooled to room temperature and concentrated in vacuo to give 420 mg of the desired product as a solid.

Workup

  1. additionis added
  2. temperatureThe reaction mixture is cooled to room temperature
  3. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-5ad2fa6e35a142d9bb153ef7d4ee1277
Source dataset
uspto-grants-1998_02
Patent number
US05719278

Reaction notes

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