Carbamic acid, ethyl ester → Ethoxycarbonyl-(1-benzotriazolyl)glycine

HRID 2338

反応式

HRID 2338 の反応式
[C:1](=[O:6])([O:3][CH2:4][CH3:5])[NH2:2].O.[C:8]([OH:12])(=[O:11])[CH:9]=O.[NH:13]1[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[N:15]=[N:14]1>C1(C)C=CC=CC=1>[CH2:4]([O:3][C:1]([N:2]([N:13]1[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[N:15]=[N:14]1)[CH2:9][C:8]([OH:12])=[O:11])=[O:6])[CH3:5]

参加物

5

反応物 3

HCID 5641Carbamic acid, ethyl esterHCID 15620607Glyoxylic acid, monohydrateHCID 178418385HCID 178418385、化合物

生成物 1

HCID 53982471Ethoxycarbonyl-(1-benzotriazolyl)glycine収率 96%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
15 °C

実験手順

Ethyl carbamate (69.0 g, 774.5 mmol), glyoxylic acid hydrate (71.3 g, 774.5 mmol) and benzotriazole (92.0 g, 774.5 mmol) were dissolved in toluene (2.3 1) and the mixture was heated with distillation for 3 h to precipitate the product. The mixture was diluted with toluene (totally 2.3 1) and stirred at 15° C. overnight. The resultant precipitate was collected by filtration, washed with toluene (160 ml) and dried to afford the title compound (196.06 g, 96%): mp. 189°-192° C.

後処理

  1. temperaturethe mixture was heated with distillation for 3 h
  2. customto precipitate the product
  3. additionThe mixture was diluted with toluene (totally 2.3 1) and
  4. filtrationThe resultant precipitate was collected by filtration
  5. washwashed with toluene (160 ml)
  6. customdried

出典と根拠

ORDレコード
ord-5df61b0f843d454b91abd7c3ea08a12b
出典データセット
uspto-grants-1998_03
特許番号
US05728829

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