Potassium Hydroxide → 955403-63-1

HRID 1172597노트

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HRID 1172597 반응식
[OH-].[K+].C([O:5][C:6](=[O:22])[CH:7]([CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[C:15]=1[F:21])C(OCC)=O)C>O>[F:21][C:15]1[C:16]([CH3:20])=[CH:17][CH:18]=[CH:19][C:14]=1[CH2:13][CH2:7][C:6]([OH:22])=[O:5]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 57659600HCID 57659600, 화합물

생성물 1

HCID 57659614955403-63-1수율 69.1%

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

Potassium hydroxide (387 mg, 6.9 mmol) was dissolved in water (8 ml) followed by the addition of 2-(2-fluoro-3-methyl-benzyl)-malonic acid diethyl ester (973 mg, 3.44 mmol). The mixture was refluxed for 5 h followed by removal of the ethanol under reduced pressure. Concentrated sulfuric acid (0.59 ml) was added to the remaining aqueous solution and refluxing was continued for 18 h. The reaction mixture was cooled to 0° C. and the precipitated product was filtered off, washed with water and dried at HV to give 433 mg (69%) of 3-(2-fluoro-3-methyl-phenyl)-propionic acid. LC-MS: tR=0.84 min; [M+H]+=183.20.

후처리

  1. temperatureThe mixture was refluxed for 5 h
  2. customfollowed by removal of the ethanol under reduced pressure
  3. additionConcentrated sulfuric acid (0.59 ml) was added to the remaining aqueous solution
  4. temperaturerefluxing
  5. filtrationthe precipitated product was filtered off
  6. washwashed with water
  7. customdried at HV

출처 및 근거

ORD 기록
ord-73d7330637ea45c59c7fa88a12a9160a
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834028B2

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