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

HRID 1720801ノート

反応式

HRID 1720801 の反応式
[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]

参加物

5

反応物 3

HCID 7291ThioglycerolHCID 8471TriethylamineHCID 11448tert-Butyl methacrylate

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-19c56e9a3c8349f9b565f6e2d1521d92
出典データセット
uspto-grants-1996_04
特許番号
US05506267

反応ノート

読み込み中…