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

HRID 974703노트

반응식

HRID 974703 반응식
[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]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 15097258HCID 15097258, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3a11d7a06f1d489ead9b27f7dc501336
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05068340

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