Potassium Hydroxide → 955403-63-1

HRID 1172597ノート

反応式

HRID 1172597 の反応式
[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]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 57659600HCID 57659600、化合物

生成物 1

HCID 57659614955403-63-1収率 69.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-73d7330637ea45c59c7fa88a12a9160a
出典データセット
uspto-grants-2010_11
特許番号
US07834028B2

反応ノート

読み込み中…