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

HRID 649407노트

반응식

HRID 649407 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

HCID 20143673HCID 20143673, 화합물수율 90.1%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fb0e2fb3c95045c197c8fbb49f6862e3
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04739066

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