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

HRID 280988ノート

反応式

HRID 280988 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

実験手順

A solution of ethyl 3-(4-thianyl)acrylate (10 g) in ethanol (150 ml) is hydrogenated over 10% palladium-carbon (9 g, 50% wet) under atmospheric pressure. After the mixture is stirred for 20 minutes at room temperature and then for 8 hours at 50° C., the catalyst is removed by filtration. To the filtrate 10% palladium carbon (9 g, 50% wet) is added and the mixture is hydrogenated at 50° C. for 1 day. After the catalyst is removed by filtration, the filtrate is evaporated in vacuo to give ethyl 3-(4-thianyl)propionate (9.1 g) as an oil.

後処理

  1. waitfor 8 hours at 50° C.
  2. customthe catalyst is removed by filtration
  3. additionTo the filtrate 10% palladium carbon (9 g, 50% wet) is added
  4. waitthe mixture is hydrogenated at 50° C. for 1 day
  5. customAfter the catalyst is removed by filtration
  6. customthe filtrate is evaporated in vacuo

出典と根拠

ORDレコード
ord-b52d3dec878d4576bc2b6b941d45033c
出典データセット
uspto-grants-1986_05
特許番号
US04591458

反応ノート

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