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

HRID 2047445노트

반응식

HRID 2047445 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2ab5f1f22a8540adb4977d1f9ea2ebee
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08592454B2

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