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

HRID 2395240ノート

反応式

HRID 2395240 の反応式
[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]

参加物

4

反応物 2

HCID 811Itaconic acidHCID 178418634HCID 178418634、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 7914Diisopropyl Ether溶媒

反応条件

温度
95 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-e04bc3ed6af646bca450e1f279a46d4b
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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