Sodium Hydroxide → 2-(Benzyloxy)propanoic acid

HRID 512809

反応式

HRID 512809 の反応式
[CH2:1]([O:8][CH:9]([CH3:14])[C:10]([O:12]C)=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>O>[CH2:1]([O:8][CH:9]([CH3:14])[C:10]([OH:12])=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応条件

温度
2.5 °C

実験手順

A mixture of residue containing methyl 2-(benzyloxy)propanoate compound of formula-12 obtained in step-a) and water (500 ml) was cooled to 0-5° C. A solution of sodium hydroxide (51.5 g) in water (375 ml) was added to reaction mixture at 0-5° C. and stirred the reaction mixture for 1 hour at the same temperature. Temperature of the reaction mixture was raised to 25-30° C. and stirred for 4 hours at this temperature. After completion of the reaction, washed the reaction mixture with dichloromethane. Both dichloromethane and aqueous layers were separated and pH of aqueous layer was adjusted to 2.5 using 50% hydrochloric acid solution. Extracted the aqueous layer with dichloromethane. Distilled off the solvent from dichloromethane layer under reduced pressure to get the title compound as a residue. The obtained residue can be taken into next step without isolation.

後処理

  1. additionA mixture of residue
  2. temperatureTemperature of the reaction mixture was raised to 25-30° C.
  3. stirringstirred for 4 hours at this temperature
  4. customAfter completion of the reaction
  5. washwashed the reaction mixture with dichloromethane
  6. customBoth dichloromethane and aqueous layers were separated
  7. extractionExtracted the aqueous layer with dichloromethane
  8. distillationDistilled off the solvent from dichloromethane layer under reduced pressure

出典と根拠

ORDレコード
ord-eb8e461d935e40faaf55fbea3460a006
出典データセット
uspto-grants-2015_08
特許番号
US09102664B2

関連ノート

読み込み中…