Methyl iodide → HCID 20301738, compound

HRID 1705997Notes

Reaction equation

HRID 1705997 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][CH2:10][CH2:9][C:8](=[O:12])[N:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:6]=2[CH:19]=1.CI.[C:22](=O)([O-])[O-].[K+].[K+]>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH3:22])[CH2:10][CH2:9][C:8](=[O:12])[N:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:6]=2[CH:19]=1

Participants

4

Reactant 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 71709Lofendazam

Product 1

HCID 20301738HCID 20301738, compound

Procedure

20.4 g 8-chloro-1-phenyl-2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one is stirred for 2 hours on a water bath with 12.8 g methyl iodide and 10 g anhydrous potassium carbonate. The inorganic material is removed by filtration under suction and the filtrate is diluted with 200 ml water. The crystalline precipitate is filtered under suction, washed with water, and recrystallized from alcohol. The yield is 20 g of the m.p.=143°-144° C. (93% of the theory).

Workup

  1. customThe inorganic material is removed by filtration under suction
  2. additionthe filtrate is diluted with 200 ml water
  3. filtrationThe crystalline precipitate is filtered under suction
  4. washwashed with water
  5. customrecrystallized from alcohol

Sources & evidence

ORD record
ord-0b83dcec888a4eb9ab956cc68bcc0c4a
Source dataset
uspto-grants-1980_06
Patent number
USRE030293

Reaction notes

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