Triethylamine → 4-(Methanesulfonyl)oxytetrahydrothiopyran

HRID 2270104ノート

反応式

HRID 2270104 の反応式
[OH:1][CH:2]1[CH2:7][CH2:6][S:5][CH2:4][CH2:3]1.[CH3:8][S:9](Cl)(=[O:11])=[O:10].C(N(CC)CC)C>C(Cl)Cl>[CH3:8][S:9]([O:1][CH:2]1[CH2:7][CH2:6][S:5][CH2:4][CH2:3]1)(=[O:11])=[O:10]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 576296Tetrahydro-2H-thiopyran-4-ol

生成物 1

HCID 124202654-(Methanesulfonyl)oxytetrahydrothiopyran

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a 300 ml methylene chloride solution of 14.6 g (0.12 mol) of 4-hydroxytetrahydrothiopyran, 11.5 ml (0.15 mol) of methanesulfonyl chloride and 25.8 ml (0.19 mol) of triethylamine were added at 0° C. and stirred at room temperature for 1 hour. The reaction mixture was diluted with methylene chloride (100 ml) and successively washing with water (100 ml) and saturated saline (100 ml), followed by drying over anhydrous sodium sulfate. The solvent was then distilled off under vacuum to obtain 24.5 g (quant.) of the above-identified compound as a slightly brown crystal.

後処理

  1. washsuccessively washing with water (100 ml) and saturated saline (100 ml)
  2. dry with materialby drying over anhydrous sodium sulfate
  3. distillationThe solvent was then distilled off under vacuum
  4. customto obtain 24.5 g (quant.) of the above-identified compound as a slightly brown crystal

出典と根拠

ORDレコード
ord-9332a5eff53840b7b73ba6a6f266a355
出典データセット
uspto-grants-2001_12
特許番号
US06331548B1

反応ノート

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