Hydrochloric Acid → 1-[3,5-Bis(trifluoromethyl)phenyl]cyclopropanecarboxylic acid

HRID 2047445ノート

反応式

HRID 2047445 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[C:5]([C:13]2([C:16]([O:18]C)=[O:17])[CH2:15][CH2:14]2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[OH-].[Na+].Cl>CO>[F:1][C:2]([F:20])([F:21])[C:3]1[CH:4]=[C:5]([C:13]2([C:16]([OH:18])=[O:17])[CH2:15][CH2:14]2)[CH:6]=[C:7]([C:9]([F:11])([F:12])[F:10])[CH:8]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21955134Methyl 1-[3,5-Bis(trifluoromethyl)phenyl]cyclopropanecarboxylate

生成物 1

HCID 219552021-[3,5-Bis(trifluoromethyl)phenyl]cyclopropanecarboxylic acid収率 81%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
60 °C

実験手順

To a solution of the compound (1.80 g) obtained in step 2 in methanol (10 mL) was added 8N aqueous sodium hydroxide solution (10 mL), and the mixture was stirred at 60° C. for 1.5 hr. The reaction mixture was cooled, and the mixture was acidified with 6N hydrochloric acid, and methanol was evaporated under reduced pressure. The residue was extracted twice with ethyl acetate, dried and concentrated under reduced pressure to give the title compound (1.39 g, 81%) as a white powder.

後処理

  1. temperatureThe reaction mixture was cooled
  2. customwas evaporated under reduced pressure
  3. extractionThe residue was extracted twice with ethyl acetate
  4. customdried
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2ab5f1f22a8540adb4977d1f9ea2ebee
出典データセット
uspto-grants-2013_11
特許番号
US08592454B2

反応ノート

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