Lithium Hydroxide → 2,2-Bis-(2-phenylsulfanyl-ethyl)-malonic acid

HRID 1830124노트

반응식

HRID 1830124 반응식
C([O:3][C:4](=[O:29])[C:5]([CH2:20][CH2:21][S:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([CH2:11][CH2:12][S:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:6]([O:8]CC)=[O:7])C.[OH-].[Li+]>C(O)C.O>[C:23]1([S:22][CH2:21][CH2:20][C:5]([CH2:11][CH2:12][S:13][C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)([C:4]([OH:29])=[O:3])[C:6]([OH:8])=[O:7])[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 694375232,2-Bis-(2-phenylsulfanyl-ethyl)-malonic acid diethyl ester

생성물 1

HCID 220539352,2-Bis-(2-phenylsulfanyl-ethyl)-malonic acid수율 115.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

반응 조건

온도
49 °C

실험 절차

A solution of 2,2-bis-(2-phenylsulfanyl-ethyl)-malonic acid diethyl ester (5.614 g) in ethanol (100 mL) was treated with lithium hydroxide (2.84 g) in water (10 mL). The reaction mixture was heated at 49° C. for 17 hours followed by 85° C. for 2 hours. The solvents were evaporated at reduced pressure to give a residue that was treated with water (100 mL) and washed with ether. The aqueous layer was cooled on ice, acidified and the product extracted with ethyl acetate. The extracts were dried over magnesium sulfate. The solvent was removed by rotary evaporation at reduced pressure to give acid 2,2-bis-(2-phenylsulfanyl-ethyl)-malonic acid (5.628 g).

후처리

  1. customThe solvents were evaporated at reduced pressure
  2. customto give a residue that
  3. washwashed with ether
  4. temperatureThe aqueous layer was cooled on ice
  5. extractionthe product extracted with ethyl acetate
  6. dry with materialThe extracts were dried over magnesium sulfate
  7. customThe solvent was removed by rotary evaporation at reduced pressure

출처 및 근거

ORD 기록
ord-b0fded355c5b4af68af6197c8aea378b
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07064123B1

반응 노트

불러오는 중…