Acetic Acid → HCID 136335633, compound

HRID 1732693Notes

Reaction equation

HRID 1732693 reaction equation
[N:1]([O-:3])=O.[Na+].[CH2:5]([O:7][C:8](=[O:29])[CH:9]=[C:10]1[CH2:16][N:15]=[C:14]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:23])[C:13]2[CH:24]=[C:25]([Cl:28])[CH:26]=[CH:27][C:12]=2[NH:11]1)[CH3:6].C(O)(=O)C>O>[CH2:5]([O:7][C:8](=[O:29])[C:9](=[N:1][OH:3])[C:10]1[CH2:16][N:15]=[C:14]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:23])[C:13]2[CH:24]=[C:25]([Cl:28])[CH:26]=[CH:27][C:12]=2[N:11]=1)[CH3:6]

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 23668193Sodium NitriteHCID 70573655HCID 70573655, compound

Product 1

HCID 136335633HCID 136335633, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Sodium nitrite, 1.5 g. (0.022 mol), was added to a solution of 6.2 g. crude 7-chloro-5-(2-chlorophenyl)-1,3-dihydro-2H-1,4-benzodiazepine-2-ylideneacetic acid ethyl ester in 75 ml. of glacial acetic acid. After stirring at room temperature for 20 minutes the reaction mixture was diluted with 200 ml. of water. The precipitated product was collected, washed with water and sucked dry to give crude product. The analytical sample was recrystallized from methylene chloride/ethanol to give light yellow crystals with mp 219°-221°.

Workup

  1. addition(0.022 mol), was added to a solution of 6.2 g
  2. additionwas diluted with 200 ml
  3. customThe precipitated product was collected
  4. washwashed with water
  5. customsucked dry
  6. customto give crude product
  7. customThe analytical sample was recrystallized from methylene chloride/ethanol
  8. customto give light yellow crystals with mp 219°-221°

Sources & evidence

ORD record
ord-8c390c3a0da64f179af54e45d73a659e
Source dataset
uspto-grants-1980_12
Patent number
US04238610

Reaction notes

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