Water → Methyl [(2-oxobutyl)sulfanyl]acetate

HRID 1061664ノート

反応式

HRID 1061664 の反応式
C(N(CC)CC)C.[OH:8][CH:9]([CH2:17][CH3:18])[CH2:10][S:11][CH2:12][C:13]([O:15][CH3:16])=[O:14].O>CS(C)=O>[O:8]=[C:9]([CH2:17][CH3:18])[CH2:10][S:11][CH2:12][C:13]([O:15][CH3:16])=[O:14]

参加物

5

反応物 3

HCID 962WaterHCID 8471TriethylamineHCID 22284251Methyl 2-(2-hydroxybutylthio)acetate

生成物 1

HCID 12353742Methyl [(2-oxobutyl)sulfanyl]acetate

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

Triethylamine (28.3 ml) is added to a solution of methyl 2-(2-hydroxybutylthio)acetate (6.00 g, Reference compound No. 35-1) in dimethyl sulfoxide (180 ml). A sulfur trioxide-pyridine complex (20.0 g) is added to the mixture, and the whole is stirred for one hour. Water is added to the reaction mixture, and the whole is stirred for 20 minutes and extracted with ethyl acetate. The extract is washed with water, 1 N hydrochloric acid and saturated brine successively and dried over anhydrous magnesium sulfate. The extract is concentrated under reduced pressure, and the resulting residue is purified by silica gel column chromatography to give the titled reference compound (5.93 g).

後処理

  1. additionA sulfur trioxide-pyridine complex (20.0 g) is added to the mixture
  2. stirringthe whole is stirred for 20 minutes
  3. extractionextracted with ethyl acetate
  4. washThe extract is washed with water, 1 N hydrochloric acid and saturated brine successively
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationThe extract is concentrated under reduced pressure
  7. customthe resulting residue is purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-041cbb27fc20401c92b6a987c39cc489
出典データセット
uspto-grants-2005_11
特許番号
US06960575B2

反応ノート

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