Thioglycerol → 6,7Dihydroxy-3methyl-4-thiaheptanoic acid t-butyl ester

HRID 1720794

반응식

HRID 1720794 반응식
[SH:1][CH2:2][CH:3]([CH2:5][OH:6])[OH:4].[C:7]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])(=[O:11])/[CH:8]=[CH:9]/[CH3:10].C(N(CC)CC)C>O>[C:13]([O:12][C:7](=[O:11])[CH2:8][CH:9]([CH3:10])[S:1][CH2:2][CH:3]([OH:4])[CH2:5][OH:6])([CH3:16])([CH3:15])[CH3:14]

참가 물질

5

반응물 3

HCID 7291ThioglycerolHCID 8471TriethylamineHCID 5463127tert-Butyl Crotonate

생성물 1

HCID 105626566,7Dihydroxy-3methyl-4-thiaheptanoic acid t-butyl ester수율 73%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

To thioglycerol (0.835 ml), t-butyl crotonate (10 ml) and triethylamine (1 ml) were added, followed by stirring at 60° C. for 48 hours. After cooling and addition of water, the reaction mixture was extracted with ethyl acetate. The extract was washed with a 5% aqueous solution of citric acid, a saturated aqueous solution of sodium hydrogen carbonate and saturated saline, and dried over anhydrous sodium sulfate, and the solvent was distilled off, to yield the title compound (1.82 g, yield 73%) as a colorless oily substance.

후처리

  1. temperatureAfter cooling
  2. extractionthe reaction mixture was extracted with ethyl acetate
  3. washThe extract was washed with a 5% aqueous solution of citric acid
  4. dry with materiala saturated aqueous solution of sodium hydrogen carbonate and saturated saline, and dried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-8f641081fb3b4fbf8f3b3c0e8fc51e3e
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05506267

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