Itaconic acid → Butanedioic acid, 2-[(acetylthio)methyl]-

HRID 2395240노트

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HRID 2395240 반응식
[C:1]([OH:9])(=[O:8])[C:2]([CH2:4][C:5]([OH:7])=[O:6])=[CH2:3].[C:10]([OH:13])(=[S:12])[CH3:11]>C(OC(C)C)(C)C>[C:10]([S:12][CH2:3][CH:2]([CH2:4][C:5]([OH:7])=[O:6])[C:1]([OH:9])=[O:8])(=[O:13])[CH3:11]

참가 물질

4

반응물 2

HCID 811Itaconic acidHCID 178418634HCID 178418634, 화합물

생성물 1

HCID 15307653Butanedioic acid, 2-[(acetylthio)methyl]-수율 91.9%

시약·촉매·용매 1

HCID 7914Diisopropyl Ether용매

반응 조건

온도
95 °C

실험 절차

400 g (3.07 mol) of itaconic acid (VIII) are added in portions within a period of approximately 30 minutes to 280 g (3.68 mol) of thioacetic acid, with simultaneous heating of the heating bath to 95° C. After 2.5 hours' stirring at 90°-100° C., the reaction mixture is cooled to room temperature and diluted with 300 ml of diisopropyl ether (DIPE), whereupon the product crystallises out within a period of approximately 12 hours. There are obtained 582 g of crystals having a melting point of 89°-91° C.

후처리

  1. temperaturethe reaction mixture is cooled to room temperature
  2. customcrystallises out within a period of approximately 12 hours

출처 및 근거

ORD 기록
ord-e04bc3ed6af646bca450e1f279a46d4b
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05814629

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