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

HRID 1769113ノート

反応式

HRID 1769113 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-58b09cce58db44e5a6faa14061ea2bdc
出典データセット
uspto-grants-1995_01
特許番号
US05380721

反応ノート

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