Thioglycerol → 6,7-Dihydroxy-2-methyl-4-thiaheptanoic acid t-butyl ester

HRID 1720801노트

반응식

HRID 1720801 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])[C:8]([CH3:10])=[CH2:9].C(N(CC)CC)C>O>[C:13]([O:12][C:7](=[O:11])[CH:8]([CH3:10])[CH2:9][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 11448tert-Butyl methacrylate

생성물 1

HCID 106344486,7-Dihydroxy-2-methyl-4-thiaheptanoic acid t-butyl ester수율 84%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

To thioglycerol (0.835 mI), t-butyl methacrylate (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 chloroform. 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 (2.11 g, yield 84%) as a colorless oily substance.

후처리

  1. temperatureAfter cooling
  2. extractionthe reaction mixture was extracted with chloroform
  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-19c56e9a3c8349f9b565f6e2d1521d92
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05506267

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