Sodium Hydroxide → HCID 10877456, 화합물

HRID 2395241노트

반응식

HRID 2395241 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 10877456HCID 10877456, 화합물수율 82.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-167c631227634bc0a1fe18afc2fa3d06
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05814629

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