Water → 2-Methyl-4-[(4-methylbenzenesulfonyl)oxy]butan-2-ol

HRID 78519

反応式

HRID 78519 の反応式
[CH3:1][C:2]([OH:7])([CH3:6])[CH2:3][CH2:4][OH:5].[C:8]1([CH3:18])[CH:13]=[CH:12][C:11]([S:14](Cl)(=[O:16])=[O:15])=[CH:10][CH:9]=1.O>N1C=CC=CC=1>[CH3:18][C:8]1[CH:13]=[CH:12][C:11]([S:14]([O:5][CH2:4][CH2:3][C:2]([OH:7])([CH3:6])[CH3:1])(=[O:16])=[O:15])=[CH:10][CH:9]=1

参加物

5

反応物 3

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 247470Isopentyldiol

生成物 1

HCID 140012952-Methyl-4-[(4-methylbenzenesulfonyl)oxy]butan-2-ol

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

To a solution of 3-methylbutane-1,3-diol (2.13 mL, 20 mmol) in pyridine (20 mL) at 0° C. was added para-toluenesulfonyl chloride (3.8 g, 20 mmol) in pyridine (10 mL) drop-wise over 15 minutes. This mixture stirred at ambient temperature for 3 hours and 35 mL H2O was added and the mixture was extracted with ethyl acetate (2×50 mL). The combined organics were washed with H2O (2×50 mL), dried over MgSO4, filtered, concentrated under reduced pressure and dried under vacuum (˜1 mm Hg) to afford the title compound. MS (ESI) m/z 276 (M+18)+.

後処理

  1. extractionthe mixture was extracted with ethyl acetate (2×50 mL)
  2. washThe combined organics were washed with H2O (2×50 mL)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customdried under vacuum (˜1 mm Hg)

出典と根拠

ORDレコード
ord-7a7fd07a31984e249677bcd4f6de1b19
出典データセット
uspto-grants-2014_09
特許番号
US08841334B2

関連ノート

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