Acetic Anhydride → HCID 11013758, compound

HRID 2393488Notes

Reaction equation

HRID 2393488 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:11]([C:12]3[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=3)=[N:10][NH:9][CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1.[C:23](OC(=O)C)(=[O:25])[CH3:24]>>[C:23]([N:9]1[CH:8]([CH3:21])[CH2:7][C:6]2[CH:22]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[C:11]([C:12]2[CH:13]=[CH:14][C:15]([N+:18]([O-:20])=[O:19])=[CH:16][CH:17]=2)=[N:10]1)(=[O:25])[CH3:24]

Participants

3

Reactant 2

HCID 7918Acetic AnhydrideHCID 11023487HCID 11023487, compound

Product 1

HCID 11013758HCID 11013758, compoundYield 88%

Procedure

0.72 g (2.2 mmoles) of 7-chloro-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine are stirred in 4 ml of acetic anhydride at 25° C. for 3 hours, then the reaction mixture is poured onto 20 ml of ice water, the crystalline product is filtered and washed with water several times. The crude product obtained is purified by suspending it in 4 ml of hot ethanol. After filtration and drying, 0.69 g (88%) of the title compound are obtained M.p.: 174°-175° C.

Workup

  1. filtrationthe crystalline product is filtered
  2. washwashed with water several times
  3. customThe crude product obtained
  4. customis purified
  5. filtrationAfter filtration
  6. customdrying

Sources & evidence

ORD record
ord-acea4f7cfb8145d7b02f73b53fb3f6f7
Source dataset
uspto-grants-1998_09
Patent number
US05807851

Reaction notes

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