Water → Benzyl 3-hydroxy-2,2-dimethylpropanoate

HRID 729595

반응식

HRID 729595 반응식
[OH-].[K+].O[C:4]([CH3:10])([CH2:8][OH:9])[C:5]([OH:7])=[O:6].[CH2:11](Br)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.O.[CH3:20]N(C=O)C>C(OCC)(=O)C>[CH2:11]([O:7][C:5](=[O:6])[C:4]([CH3:10])([CH3:20])[CH2:8][OH:9])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

7

반응물 5

HCID 962WaterHCID 6228DimethylformamideHCID 7498Benzyl BromideHCID 14797Potassium HydroxideHCID 5607812-Methylglyceric acid

생성물 1

HCID 18922595Benzyl 3-hydroxy-2,2-dimethylpropanoate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

반응 조건

온도
100 °C

실험 절차

Add potassium hydroxide (486.7 mmol, 32.1 g) over a solution of 2,3-dihydroxy-2-methyl-propionic acid (423.2 mmol, 50 g) in 300 mL of DMF. Stir for 1 hour at 100° C. Then add benzyl bromide (584.04 mmol, 69.46 mL) and stir overnight. Cool down the mixture and dilute with ethyl acetate. Wash organic layer with water. Wash aqueous layer with ethyl acetate several times. Combine organic layers and dry over sodium sulfate, filter and concentrate under reduced pressure. 1H NMR (CDCl3, 300 MHz): δ ppm :7.36-7.32 (m, 5H), 5.1 (s, 2H), 3.5 (s, 2H), 1.21 (s, 6H).

후처리

  1. temperatureCool down the mixture
  2. dry with materialCombine organic layers and dry over sodium sulfate
  3. filtrationfilter
  4. concentrationconcentrate under reduced pressure

출처 및 근거

ORD 기록
ord-dbc2e2a6b2624307b2c09ace19340ad6
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582638B2

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