Triethylamine → HCID 13657069、化合物

HRID 979325

反応式

HRID 979325 の反応式
[Cl:1][C:2]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:14]([O-:16])=[O:15])=[C:9]([CH:13]=1)[C:10](Cl)=[O:11].[C:25]([O:35][CH2:36][CH3:37])(=[O:34])[CH:26]([CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])[OH:27].C(N(CC)CC)C>CC(C)=O.O>[Cl:1][C:2]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:6]=[CH:7][C:8]([N+:14]([O-:16])=[O:15])=[C:9]([CH:13]=1)[C:10]([O:27][CH:26]([C:25]([O:35][CH2:36][CH3:37])=[O:34])[CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])=[O:11]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 24197Diethyl malateHCID 30177655-(2-Chloro-4-(trifluoromethyl)phenoxy)-2-nitrobenzoyl chloride

生成物 1

HCID 13657069HCID 13657069、化合物収率 66.7%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒3 回HCID 962Water溶媒

実験手順

To a stirred solution of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoyl 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 3.56 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-c3b3c7d9e0284cfe931dcb2aa93c815f
出典データセット
uspto-grants-1987_05
特許番号
US04667052

関連ノート

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