2-Thiopheneacetic acid → Methyl 2-acetylthio-3-methylbutanoate

HRID 1609440

反応式

HRID 1609440 の反応式
[CH3:1][C:2](C)([O-:4])C.[K+].[S:7]1C=CC=C1CC(O)=O.Br[CH:17]([CH:22]([CH3:24])[CH3:23])[C:18]([O:20][CH3:21])=[O:19]>CN(C)C=O.CCOCC>[C:2]([S:7][CH:17]([CH:22]([CH3:24])[CH3:23])[C:18]([O:20][CH3:21])=[O:19])(=[O:4])[CH3:1]

参加物

6

反応物 3

HCID 159702-Thiopheneacetic acidHCID 228837Methyl 2-bromo-3-methylbutanoateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 20081438Methyl 2-acetylthio-3-methylbutanoate

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
10 °C

実験手順

Potassium tert-butoxide (20.4 g) was added portionwise with stirring and cooling to thiolacetic acid (13.85 g) in dry dimethylformamide (150 ml). Stirring was continued for five minutes, then methyl 2-bromo-3-methylbutanoate (32.3 g) was added with ice-cooling (about 10° C. internal temperature). After stirring at room temperature overnight, the reaction mixture was diluted with ether (about 1 liter), washed with water (3 times), dried over magnesium sulfate and run down under vacuum. The title product was obtained as an orange oil, 29.2 g (93%).

後処理

  1. stirringStirring
  2. stirringAfter stirring at room temperature overnight
  3. washwashed with water (3 times)
  4. dry with materialdried over magnesium sulfate

出典と根拠

ORDレコード
ord-2e2d480d1ef44d93bef10395f92d73ce
出典データセット
uspto-grants-1995_03
特許番号
US05401710

関連ノート

読み込み中…