Acetone → HCID 13657069、化合物

HRID 745674ノート

反応式

HRID 745674 の反応式
[Cl:1][C:2]1[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[CH:16][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:13]([O-:15])=[O:14])=[C:9]([CH:12]=1)[CH2:10]Cl.[C:24]([O:34][CH2:35][CH3:36])(=[O:33])[CH:25]([CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])[OH:26].C(N(CC)CC)C.CC(C)=[O:46]>O>[CH2:35]([O:34][C:24]([CH:25]([O:26][C:10](=[O:46])[C:9]1[CH:12]=[C:5]([O:4][C:3]2[CH:16]=[CH:17][C:18]([C:20]([F:23])([F:22])[F:21])=[CH:19][C:2]=2[Cl:1])[CH:6]=[CH:7][C:8]=1[N+:13]([O-:15])=[O:14])[CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])=[O:33])[CH3:36]

参加物

6

反応物 4

HCID 180Acetone3 回HCID 8471TriethylamineHCID 24197Diethyl malateHCID 13090781HCID 13090781、化合物

生成物 1

HCID 13657069HCID 13657069、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred solution of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzyl chloride (3.8 g, 0.01 mole) in acetone (10 ml) was successively added diethyl DL malate (1.9 g, 0.01 mole) in acetone (10 ml) and triethylamine (1.01 g, 0.01 mole) in acetone (5 ml). A white precipitate quickly formed. The reaction was heated to reflux for 24 hours. Upon cooling, the reaction was poured in water (75 ml) and extracted twice with methylene chloride (25 ml@). The combined organic extracts were successively washed with 5% sodium hydroxide and brine solutions. The dried solution was stripped of solvent to give 3.5 g of an amber oil.

後処理

  1. customA white precipitate quickly formed
  2. temperatureThe reaction was heated
  3. temperatureto reflux for 24 hours
  4. temperatureUpon cooling
  5. extractionextracted twice with methylene chloride (25 ml@)
  6. washThe combined organic extracts were successively washed with 5% sodium hydroxide and brine solutions

出典と根拠

ORDレコード
ord-b14a83937ea54b66b9bb63b80b93e972
出典データセット
uspto-grants-1986_07
特許番号
US04599442

反応ノート

読み込み中…