Benzene → HCID 13505928, 화합물

HRID 279775노트

반응식

HRID 279775 반응식
C([C:3](CC)(Cl)[C:4]([N:6]([CH:18]([C:22]([O-:24])=[O:23])[C:19]([O-:21])=[O:20])[CH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][C:9]=1[O:16][CH3:17])=[O:5])C.[CH2:28](N(CC)CC)[CH3:29].[CH:35]1C=CC=C[CH:36]=1>>[CH2:28]([O:21][C:19]([C:18]1([C:22]([O:24][CH2:35][CH3:36])=[O:23])[CH2:3][C:4](=[O:5])[N:6]1[CH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][C:9]=1[O:16][CH3:17])=[O:20])[CH3:29]

참가 물질

4

반응물 3

HCID 241BenzeneHCID 8471TriethylamineHCID 131714654HCID 131714654, 화합물

생성물 1

HCID 13505928HCID 13505928, 화합물수율 89%

실험 절차

A mixture of 35 g (0.087 mole) of diethyl-[N-(2,4-dimethoxy-benzyl)-N-(chloro-acetyl)-amino-malonate], 15.9 ml (11.4 g, 0.113 mole) of triethylamine and 200 ml of anhydrous benzene is heated to boiling for 8 hours. The mixture is extracted successively with 100 ml of water, 100 ml of diluted hydrochloric acid and 100 ml of water, the benzene phase is dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated. Thus 28,4 g of diethyl-[1-(2,4-dimethoxy-benzyl)-4-oxo-2,2-azetidine-dicarboxylate] are obtained, yield: 89%. B.p.: 175°-180° C./0.1 Hgmm.

후처리

  1. temperatureis heated
  2. extractionThe mixture is extracted successively with 100 ml of water, 100 ml of diluted hydrochloric acid and 100 ml of water
  3. dry with materialthe benzene phase is dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customthe filtrate is evaporated

출처 및 근거

ORD 기록
ord-1bb1e10fd79644a2baee655155b14b0b
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587049

반응 노트

불러오는 중…