Sodium Hydroxide → HCID 10877456、化合物

HRID 2395241ノート

反応式

HRID 2395241 の反応式
C([S:4][CH2:5][CH:6]([CH2:10][C:11]([OH:13])=[O:12])[C:7]([OH:9])=[O:8])(=O)C.[OH-].[Na+]>O>[SH:4][CH2:5][CH:6]([CH2:10][C:11]([OH:13])=[O:12])[C:7]([OH:9])=[O:8]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 15307653Butanedioic acid, 2-[(acetylthio)methyl]-

生成物 1

HCID 10877456HCID 10877456、化合物収率 82.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

582 g (2.85 mol) of acetylthiomethylbutanedioic acid (VII) are added, under nitrogen and while cooling with ice, to a solution of 570 g (14.25 mol) of NaOH in 3 litres of water (exothermic reaction). After 15 hours' stirring at room temperature, the reaction mixture is acidified to pH 1 with concentrated hydrochloric acid and extraction is carried out with ether. The combined organic phases are dried over sodium sulfate and concentrated to dryness, and the crystalline residue is washed with 200 ml of cold dichloromethane. There are obtained 385 g of crystals having a melting point of 107°-108.5° C.

後処理

  1. extractionthe reaction mixture is acidified to pH 1 with concentrated hydrochloric acid and extraction
  2. dry with materialThe combined organic phases are dried over sodium sulfate
  3. concentrationconcentrated to dryness
  4. washthe crystalline residue is washed with 200 ml of cold dichloromethane

出典と根拠

ORDレコード
ord-167c631227634bc0a1fe18afc2fa3d06
出典データセット
uspto-grants-1998_09
特許番号
US05814629

反応ノート

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