Water → 4,4,4-Trifluoro-2,2-dimethylbutanoic acid

HRID 238773노트

반응식

HRID 238773 반응식
[F:1][C:2]([F:13])([F:12])[CH2:3][C:4]([CH3:11])([CH3:10])[C:5]([O:7]CC)=[O:6].[Li+].[OH-].O>CO>[F:1][C:2]([F:12])([F:13])[CH2:3][C:4]([CH3:10])([CH3:11])[C:5]([OH:7])=[O:6]

참가 물질

5

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 9990309Ethyl 2,2-dimethyl-4,4,4-trifluorobutanoate

생성물 1

HCID 100579374,4,4-Trifluoro-2,2-dimethylbutanoic acid수율 101.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of ethyl 4,4,4-trifluoro-2,2-dimethylbutanoate (426 mg, 2.15 mmol) in MeOH (15 mL) was added a solution of LiOH in H2O (2 N, 5.35 mL, 10.75 mmol). The reaction mixture was stirred at room temperature overnight. The reaction was concentrated and the resulting mixture was diluted with DCM and washed with 3 N HCl. The aqueous layer was extracted twice with DCM. The combined organic layers were dried over MgSO4, filtered and concentrated to yield 4,4,4-trifluoro-2,2-dimethylbutanoic acid as a colorless oil (370 mg, 100% yield). 1H NMR (400 MHz, CDCl3) ppm 1.35 (s, 6H), 2.48 (ABqt, J=12 Hz, 2H).

후처리

  1. concentrationThe reaction was concentrated
  2. additionthe resulting mixture was diluted with DCM
  3. washwashed with 3 N HCl
  4. extractionThe aqueous layer was extracted twice with DCM
  5. dry with materialThe combined organic layers were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-04c7059ce90b455f8210facacb052de5
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642576B2

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