1,1'-Carbonyldiimidazole → 1,2,4,5-Tetrahydro-4-methyl-1-phenyl-3H-2,4-benzodiazepin-3-one

HRID 54967노트

반응식

HRID 54967 반응식
[CH3:1][NH:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH:10]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[NH2:11].[C:18](N1C=CN=C1)(N1C=CN=C1)=[O:19]>C(Cl)(Cl)Cl>[CH3:1][N:2]1[C:18](=[O:19])[NH:11][CH:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH2:3]1

참가 물질

4

반응물 2

HCID 682631,1'-CarbonyldiimidazoleHCID 149782392-[(Methylamino)methyl]-alpha-phenylbenzenemethanamine

생성물 1

HCID 149782501,2,4,5-Tetrahydro-4-methyl-1-phenyl-3H-2,4-benzodiazepin-3-one수율 71.1%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of 32.8 g (145 mmol) of 2-[(methylamino)methyl]-α-phenylbenzenemethanamine in 215 mL of chloroform was treated with 25.9 g (159 mmol) of carbonyldiimidazole. The reaction was stirred at room temperature for 19 hours, washed four times with water, dried over sodium sulfate and stripped in vacuo. The gummy residue was triturated in and recrystallized from ethyl acetate to yield 26 g (71%) of product, mp 198-199.

후처리

  1. washwashed four times with water
  2. dry with materialdried over sodium sulfate
  3. customThe gummy residue was triturated in and
  4. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-f500d8a17ba74cfcbc33c035f86486e4
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624922

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