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

HRID 54967ノート

反応式

HRID 54967 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-f500d8a17ba74cfcbc33c035f86486e4
出典データセット
uspto-grants-1997_04
特許番号
US05624922

反応ノート

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