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

HRID 386338ノート

反応式

HRID 386338 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8cbe1a62429743d181417fb5887de095
出典データセット
uspto-grants-2013_02
特許番号
US08372307B2

反応ノート

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