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Hydrochloric Acid → 1-(4-(Trifluoromethoxy)phenyl)cyclopropanecarboxylic acid

HRID 1666694
ノート
印刷プレビュー

反応式

HRID 1666694 の反応式
NN1CCCC1.[F:7][C:8]([F:23])([F:22])[O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2([C:19](N)=[O:20])[CH2:18][CH2:17]2)=[CH:12][CH:11]=1.[OH-:24].[Na+].Cl>CO>[F:7][C:8]([F:23])([F:22])[O:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2([C:19]([OH:24])=[O:20])[CH2:18][CH2:17]2)=[CH:12][CH:11]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 279461-PyrrolidinamineHCID 57970159HCID 57970159、化合物

生成物 1

HCID 459257321-(4-(Trifluoromethoxy)phenyl)cyclopropanecarboxylic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
78 °C

実験手順

A mixture of 1-(4-trifluoromethoxyphenyl)cyclopropanecarbonitrile (4.0 g), 25% aqueous sodium hydroxide (0.46 mL), 30% aqueous hydrogen peroxide (25 mL), and methanol (100 mL) was heated at 55° C. for 1 h with stirring. The reaction mixture was concentrated under reduced pressure, the precipitated crystals were collected by filtration, to obtain white solid 1-(4-(trifluoromethoxy)phenyl)cyclopropanecarbamide (4.5 g). (3) A mixture of 1-(4-trifluoromethoxyphenyl)cyclopropanecarbamide (4.5 g), 15% aqueous sodium hydroxide (150 mL), and methanol (60 mL) was heated at 78° C. for 18 h with stirring. The reaction mixture was left stand for cooling, then the reaction solution was adjusted to pH 2 using 15% hydrochloric acid and concentrated under reduced pressure. The precipitated crystals were collected by filtration to obtain white solid 1-(4-(trifluoromethoxy)phenyl)cyclopropanecarboxylic acid (4.5 g).

後処理

  1. waitThe reaction mixture was left stand
  2. temperaturefor cooling
  3. concentrationconcentrated under reduced pressure
  4. filtrationThe precipitated crystals were collected by filtration

出典と根拠

ORDレコード
ord-bd54535b29eb4a03a597ddecc8df4e78
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044068B2

反応ノート

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