Propionyl chloride → HCID 44211248、化合物

HRID 52053

反応式

HRID 52053 の反応式
[C:1](Cl)(=[O:4])[CH2:2][CH3:3].[N:6]1([CH2:12][C:13]2[CH:18]=[CH:17][N:16]=[C:15]([O:19][CH2:20]/[CH:21]=[CH:22]\[CH2:23][NH:24][C:25](=[O:31])[CH2:26][S:27][CH2:28][CH2:29][OH:30])[CH:14]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.C(=O)([O-])O.[Na+]>N1C=CC=CC=1>[N:6]1([CH2:12][C:13]2[CH:18]=[CH:17][N:16]=[C:15]([O:19][CH2:20]/[CH:21]=[CH:22]\[CH2:23][NH:24][C:25](=[O:31])[CH2:26][S:27][CH2:28][CH2:29][O:30][C:1](=[O:4])[CH2:2][CH3:3])[CH:14]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1

参加物

5

反応物 3

HCID 62324Propionyl chlorideHCID 516892Sodium BicarbonateHCID 67725880N-[4-(4-piperidinomethyl-2-pyridyloxy)-cis-2-butenyl]-2-(2-hydroxyethylthio)acetamide

生成物 1

HCID 44211248HCID 44211248、化合物収率 85%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

0.09 ml of propionyl chloride was added to a mixture of 0.40 g of N-[4-(4-piperidinomethyl-2-pyridyloxy) -cis-2-butenyl]-2-(2-hydroxyethylthio)acetamide (prepared as described in Example 1) and 1.02 ml of pyridine, and the resulting mixture was allowed to stand at room temperature for 2 hours. At the end of this time, the reaction mixture was poured into ice-water, and a saturated aqueous solution of sodium hydrogencarbonate was added to the resulting mixture, after which it was extracted with chloroform. The extract was concentrated by evaporation under reduced pressure and the residue was purified by column chromatography through silica gel, using a 1:19 by volume mixture of methanol and ethyl acetate as the eluent, to give 0.39 g (yield 85%) of the title compound as an oil.

後処理

  1. extractionafter which it was extracted with chloroform
  2. concentrationThe extract was concentrated by evaporation under reduced pressure
  3. customthe residue was purified by column chromatography through silica gel
  4. additionby volume mixture of methanol and ethyl acetate as the eluent

出典と根拠

ORDレコード
ord-0d44a03b9b0e4691a156f7a6265534b7
出典データセット
uspto-grants-1997_04
特許番号
US05616579

関連ノート

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