Propionyl chloride → HCID 44211248, 화합물

HRID 52053

반응식

HRID 52053 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 44211248HCID 44211248, 화합물수율 85%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0d44a03b9b0e4691a156f7a6265534b7
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616579

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