Benzene → HCID 13505928、化合物

HRID 279775ノート

反応式

HRID 279775 の反応式
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]

参加物

4

反応物 3

HCID 241BenzeneHCID 8471TriethylamineHCID 131714654HCID 131714654、化合物

生成物 1

HCID 13505928HCID 13505928、化合物収率 89%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1bb1e10fd79644a2baee655155b14b0b
出典データセット
uspto-grants-1986_05
特許番号
US04587049

反応ノート

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