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Water → HCID 13314712、化合物

HRID 543572
ノート
印刷プレビュー

反応式

HRID 543572 の反応式
[CH3:1][C:2]1([C:5]([OH:7])=O)[CH2:4][CH2:3]1.[Cl:8][C:9]1[CH:10]=[C:11]([CH:13]=[CH:14][C:15]=1[O:16][CH2:17][C:18]([F:21])([F:20])[F:19])[NH2:12].O>N1C=CC=CC=1>[Cl:8][C:9]1[CH:10]=[C:11]([NH:12][C:5]([C:2]2([CH3:1])[CH2:4][CH2:3]2)=[O:7])[CH:13]=[CH:14][C:15]=1[O:16][CH2:17][C:18]([F:20])([F:21])[F:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 813261-Methylcyclopropanecarboxylic acidHCID 133055253-Chloro-4-(2,2,2-trifluoroethoxy)aniline

生成物 1

HCID 13314712HCID 13314712、化合物収率 82.9%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

To a solution of 1-methylcyclopropanecarboxylic acid (1.8 g) in pyridine (50 ml), a solution of 3-chloro-4-(2,2,2-trifluoroethoxy)aniline (2.3 g) in pyridine (10 ml) cooled with ice was dropwise added while stirring. After stirring at room temperature for 10 hours, the reaction mixture was admixed with water and extracted with ether. The extract was washed with 1 N hydrochloric acid, sodium hydrogen carbonate solution and saturated sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated. The crude crystals (2.8 g) were recrystallized from ethanol to give N-(3-chloro-4-(2,2,2-trifluoroethoxy)phenyl)-1-methylcyclopropanecarboxamide (2.6 g). M.P., 95°-96° C.

後処理

  1. additionwas dropwise added
  2. stirringAfter stirring at room temperature for 10 hours
  3. extractionextracted with ether
  4. washThe extract was washed with 1 N hydrochloric acid, sodium hydrogen carbonate solution and saturated sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe crude crystals (2.8 g) were recrystallized from ethanol

出典と根拠

ORDレコード
ord-87150c4725c24e0a9f9f199c45308877
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04447260

反応ノート

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