2-Propenoic acid, 3-(tetrahydro-2H-thiopyran-4-yl)-, ethyl ester → HCID 20143673、化合物

HRID 649407ノート

反応式

HRID 649407 の反応式
[S:1]1[CH2:6][CH2:5][CH:4]([CH:7]=[CH:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:3][CH2:2]1>C(O)C.[C].[Pd]>[S:1]1[CH2:6][CH2:5][CH:4]([CH2:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:3][CH2:2]1

参加物

4

反応物 1

HCID 537977722-Propenoic acid, 3-(tetrahydro-2H-thiopyran-4-yl)-, ethyl ester

生成物 1

HCID 20143673HCID 20143673、化合物収率 90.1%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

In 150 ml of ethanol is dissolved 10 g of ethyl 3-(4-thianyl)acrylate, and a catalytic reduction reaction is carried out at ordinary temperature and at atmospheric pressure using 9 g of 10% palladium-carbon (50% in water) as a catalyst. The reaction mixtuure is stirred at room temperature for 20 minutes and at 50° C. for 8 hours, and the catalyst is removed by filtration. Nine (9) g of 10% palladium-carbon (50% in water) is added anew to the filtrate, followed by stirring at 50° C. for one day. The catalyst is removed by filtration, and the filtrate is concentrated under reduced pressure to give 9.1 g of ethyl 3-(4-thianyl)propionate as an oily material.

後処理

  1. customa catalytic reduction reaction
  2. customthe catalyst is removed by filtration
  3. additionNine (9) g of 10% palladium-carbon (50% in water) is added anew to the filtrate
  4. stirringby stirring at 50° C. for one day
  5. customThe catalyst is removed by filtration
  6. concentrationthe filtrate is concentrated under reduced pressure

出典と根拠

ORDレコード
ord-fb0e2fb3c95045c197c8fbb49f6862e3
出典データセット
uspto-grants-1988_04
特許番号
US04739066

反応ノート

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