Ethyl orthoformate → Ro 14-7437

HRID 67318

反応式

HRID 67318 の反応式
[NH2:1][C:2](=[C:8]1[CH2:14][N:13]([CH3:15])[C:12](=[O:16])[C:11]2[CH:17]=[CH:18][CH:19]=[CH:20][C:10]=2[NH:9]1)[C:3]([O:5][CH2:6][CH3:7])=[O:4].[CH:21](OCC)(OCC)OCC>C1(C)C=CC=CC=1>[CH3:15][N:13]1[C:12](=[O:16])[C:11]2[CH:17]=[CH:18][CH:19]=[CH:20][C:10]=2[N:9]2[CH:21]=[N:1][C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[C:8]2[CH2:14]1

参加物

4

反応物 2

HCID 31214Ethyl orthoformateHCID 70541641ethyl alpha-amino-1,3,4,5-tetrahydro-4-methyl-5-oxo-2H-1,4-benzodiazepin-2-ylidene-acetate

生成物 1

HCID 127597Ro 14-7437

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1.10 g of ethyl α-amino-1,3,4,5-tetrahydro-4-methyl-5-oxo-2H-1,4-benzodiazepin-2-ylidene-acetate are dissolved in 15 ml of toluene and treated with 1.0 ml of triethyl orthoformate. The mixture is heated to reflux for 50 minutes, subsequently cooled and evaporated in vacuo. The crystalline residue is suspended in 25 ml of ethyl acetate, filtered off and dried. There is obtained ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]-benzodiazepine-3-carboxylate of melting point 165° C.

後処理

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 50 minutes
  3. temperaturesubsequently cooled
  4. customevaporated in vacuo
  5. filtrationfiltered off
  6. customdried

出典と根拠

ORDレコード
ord-6282bb24c0b34c5584d9bba722813b52
出典データセット
uspto-grants-1982_08
特許番号
US04346030

関連ノート

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