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

HRID 2405152ノート

反応式

HRID 2405152 の反応式
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

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 46220010Ethyl (4-bromophenyl)(difluoro)acetate2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
25 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-dcfb8239e3e44a82845b89ed7f52fb60
出典データセット
uspto-grants-2014_08
特許番号
US08802886B2

反応ノート

読み込み中…