Hydrochloric Acid → 2-(4-bromophenyl)-2,2-difluoroacetic acid

HRID 2405152노트

반응식

HRID 2405152 반응식
C([O:3][C:4](=[O:15])[C:5]([C:8]1[CH:13]=[CH:12][C:11]([Br:14])=[CH:10][CH:9]=1)([F:7])[F:6])C.C([O-])([O-])=O.[K+].[K+].Cl>CN(C=O)C>[Br:14][C:11]1[CH:12]=[CH:13][C:8]([C:5]([F:6])([F:7])[C:4]([OH:15])=[O:3])=[CH:9][CH:10]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 46220010Ethyl (4-bromophenyl)(difluoro)acetate2회

생성물 1

HCID 287403152-(4-bromophenyl)-2,2-difluoroacetic acid

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
25 °C

실험 절차

According to the above-described scheme, 2-(4-bromophenyl)-2,2-difluoroacetic acid ethyl ester (Compound 2f; 279.1 mg, 1.0 mmol), 1N K2CO3 solution (3.0 mL) and DMF (3.0 mL) were put into an eggplant flask, and the mixture was stirred at 25° C. for 18 hours. After the reaction, the reaction mixture was neutralized with 5% HCl solution, extracted with ethyl acetate and washed with water, and an organic layer was dried with anhydrous sodium sulfate. Ethyl acetate was distilled away under reduced pressure, and by carrying out purification by silica gel column chromatography, 2-(4-bromophenyl)-2,2-difluoroacetic acid (Compound 4f) was obtained with a yield of 85%.

후처리

  1. customwere put into an eggplant flask
  2. customAfter the reaction
  3. extractionextracted with ethyl acetate
  4. washwashed with water
  5. dry with materialan organic layer was dried with anhydrous sodium sulfate
  6. distillationEthyl acetate was distilled away under reduced pressure
  7. custompurification by silica gel column chromatography

출처 및 근거

ORD 기록
ord-dcfb8239e3e44a82845b89ed7f52fb60
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802886B2

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