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

HRID 2338

반응식

HRID 2338 반응식
[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]

참가 물질

5

반응물 3

HCID 5641Carbamic acid, ethyl esterHCID 15620607Glyoxylic acid, monohydrateHCID 178418385HCID 178418385, 화합물

생성물 1

HCID 53982471Ethoxycarbonyl-(1-benzotriazolyl)glycine수율 96%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
15 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5df61b0f843d454b91abd7c3ea08a12b
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728829

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