Methyl iodide → HCID 20542067, compound

HRID 2286164Notes

Reaction equation

HRID 2286164 reaction equation
[C:1](=[O:4])([O-])[O-].[K+].[K+].[C:7]([C:10]1[CH:11]=[CH:12][C:13]2[NH:19][C:18](=O)[CH:17]([CH3:21])[N:16]=[C:15]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[F:28])[C:14]=2[CH:29]=1)(=[O:9])[CH3:8].CI>CC(C)=O>[C:7]([C:10]1[CH:11]=[CH:12][C:13]2[N:19]([CH3:18])[C:1](=[O:4])[CH:17]([CH3:21])[N:16]=[C:15]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[F:28])[C:14]=2[CH:29]=1)(=[O:9])[CH3:8]

Participants

5

Procedure

7.15 g of potassium carbonate are added to a solution of 7.15 g (23.04 mmol) of 7-acetyl-5-(o-fluorophenyl)-1,3-dihydro-3-methyl-2H-1,4-benzodiazepin-2-one and 15 ml of methyl iodide in 300 ml of acetone and the mixture is stirred at room temperature for 21 hours. The insoluble material is filtered off and the solution is evaporated in vacuo. The residue is taken up in methylene chloride, washed with water, dried and evaporated. From cyclohexane there is obtained 7-acetyl-5-(o-fluorophenyl)-1,3-dihydro-1,3-dimethyl-2H-1,4-benzodiazepin-2-one of melting point 65°.

Workup

  1. filtrationThe insoluble material is filtered off
  2. customthe solution is evaporated in vacuo
  3. washwashed with water
  4. customdried
  5. customevaporated

Sources & evidence

ORD record
ord-711740dca1a0453ab65deb4c41c93bd3
Source dataset
uspto-grants-1982_04
Patent number
US04327026

Reaction notes

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