Pyridine → Ethyl 2-(((benzyloxy)carbonyl)amino)-2-cyanoacetate

HRID 256598

반응식

HRID 256598 반응식
[CH2:1]([O:3][C:4](=[O:9])[CH:5]([NH2:8])[C:6]#[N:7])[CH3:2].N1C=CC=CC=1.[CH2:16]([O:23][C:24](Cl)=[O:25])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O>[CH2:1]([O:3][C:4](=[O:9])[CH:5]([NH:8][C:24]([O:23][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:25])[C:6]#[N:7])[CH3:2]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 10387Benzyl chloroformateHCID 288716Ethyl 2-amino-2-cyanoacetate

생성물 1

HCID 9943163Ethyl 2-(((benzyloxy)carbonyl)amino)-2-cyanoacetate수율 60.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred mixture of 2-amino-2-cyanoacetic acid ethyl ester (19.7 g) and pyridine (12.2 g) in water (123 ml) was added portionwise benzyloxycarbonyl chloride (27.9 g) under ice cooling. The resulting mixture was stirred under ice cooling for 1 hour. Precipitated crystals were collected, washed thoroughly with water, and recrystallized from ethanol to give the title compound (24.2 g, 60.2%) as colorless crystals, mp 111°-112° C.

후처리

  1. customPrecipitated crystals
  2. customwere collected
  3. washwashed thoroughly with water
  4. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-4ea026a1293a48e196c3c781eb05705b
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258382

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