Methacrylic Acid → 4-Propyl-cyclohexanecarboxylic acid 2,2-dimethyl-3-(2-methyl-acryloyloxy)-propyl ester

HRID 386338노트

반응식

HRID 386338 반응식
Br[CH2:2][C:3]([CH3:18])([CH3:17])[CH2:4][O:5][C:6]([CH:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][CH3:16])[CH2:10][CH2:9]1)=[O:7].[C:19]([OH:24])(=[O:23])[C:20]([CH3:22])=[CH2:21].C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[CH3:17][C:3]([CH3:18])([CH2:2][O:24][C:19](=[O:23])[C:20]([CH3:22])=[CH2:21])[CH2:4][O:5][C:6]([CH:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][CH3:16])[CH2:10][CH2:9]1)=[O:7]

참가 물질

5

반응물 3

HCID 4093Methacrylic AcidHCID 11430Potassium CarbonateHCID 592890294-Propyl-cyclohexanecarboxylic acid 3-bromo-2,2-dimethyl-propyl ester

생성물 1

HCID 592890974-Propyl-cyclohexanecarboxylic acid 2,2-dimethyl-3-(2-methyl-acryloyloxy)-propyl ester

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

4-Propyl-cyclohexanecarboxylic acid 3-bromo-2,2-dimethyl-propyl ester (4.3 g, 13.3 mmol), methacrylic acid (3.4 g, 39.9 mmol) and potassium carbonate (6.9 g, 50.0 mmol) are stirred at 100° C. in dimethyl sulphoxide (100 ml) for 3d. A solid precipitate is removed by filtration and washed with diethyl ether. The filtrate is washed with water, removed, dried and evaporated to dryness. Purification is achieved by flash column chromatography using petrol as eluant to give 22 as a liquid.

후처리

  1. customA solid precipitate is removed by filtration
  2. washwashed with diethyl ether
  3. washThe filtrate is washed with water
  4. customremoved
  5. customdried
  6. customevaporated to dryness
  7. customPurification

출처 및 근거

ORD 기록
ord-8cbe1a62429743d181417fb5887de095
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372307B2

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