Potassium Hydroxide → Ethyl hydrogen 2-[5-(2-methoxyethoxy)methoxypentyl]malonate

HRID 974703ノート

反応式

HRID 974703 の反応式
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH:13]([C:19]([O:21]CC)=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15].[OH-].[K+]>C(O)C>[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH:13]([C:19]([OH:21])=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 15097258HCID 15097258、化合物

生成物 1

HCID 15097259Ethyl hydrogen 2-[5-(2-methoxyethoxy)methoxypentyl]malonate収率 81%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1.029 g of diethyl 2-[5-(2-methoxyethoxy)methoxypentyl]malonate (prepared as described in Preparation 41) dissolved in ethanol (1.5 ml) was added an aqueous solution (1.5 ml) containing potassium hydroxide (0.203 g) whilst ice-cooling. The reaction mixture was stirred at room temperature for 5 hours, after which it was washed with diethyl ether. The aqueous layer was adjusted to a pH value of 2 by adding 10% aqueous hydrochloric acid, and it was then extracted four times with methylene chloride. The combined extracts were dried and concentrated by evaporation under reduced pressure. The oily residue (0.94 g) was subjected to column chromatography through silica gel (20 g) and the title compound (0.764 g) Was obtained, as a colorless oil, from the fractions eluted with mixtures of hexane and ethyl acetate ranging from 2:1 to 1:1 by volume.

後処理

  1. temperaturecooling
  2. washafter which it was washed with diethyl ether
  3. additionby adding 10% aqueous hydrochloric acid, and it
  4. extractionwas then extracted four times with methylene chloride
  5. customThe combined extracts were dried
  6. concentrationconcentrated by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-3a11d7a06f1d489ead9b27f7dc501336
出典データセット
uspto-grants-1991_11
特許番号
US05068340

反応ノート

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