Methyl iodide → HCID 20301738, compound

HRID 2419995Notes

Reaction equation

HRID 2419995 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-9990ba8bdda844e5811b17438fcdb7bc
Source dataset
uspto-grants-1978_08
Patent number
US04108852

Reaction notes

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