Water → HCID 58452683, 화합물

HRID 70719

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HRID 70719 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]([C:9]1[CH:14]=[CH:13][C:12]([CH:15](OCC2CCCC2)[C:16]2[N:21]=[C:20]([O:22]C)[C:19]([Cl:24])=[CH:18][CH:17]=2)=[CH:11][CH:10]=1)([CH3:8])([CH3:7])[CH3:6].O.[CH:33]1([SH:38])[CH2:37][CH2:36][CH2:35][CH2:34]1>>[C:5]([C:9]1[CH:10]=[CH:11][C:12]([CH:15]([S:38][CH:33]2[CH2:37][CH2:36][CH2:35][CH2:34]2)[C:16]2[NH:21][C:20](=[O:22])[C:19]([Cl:24])=[CH:18][CH:17]=2)=[CH:13][CH:14]=1)([CH3:6])([CH3:7])[CH3:8]

참가 물질

5

반응물 4

HCID 962WaterHCID 15510CyclopentanethiolHCID 6451240Aluminum(III) ChlorideHCID 673980526-[(4-Tert-butylphenyl)(cyclopentylmethoxy)methyl]-3-chloro-2-methoxypyridine

생성물 1

HCID 58452683HCID 58452683, 화합물수율 25%

반응 조건

온도
40 °C

실험 절차

Aluminum chloride (66 mg) was added to a solution of 6-[(4-tert-butylphenyl)(cyclopentylmethoxy)methyl]-3-chloro-2-methoxypyridine (64 mg) in cyclopentanethiol (1 mL) under ice-cooling, and then the mixture was stirred at 40° C. for two hours. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and filtered, after which the solvent was evaporated under reduced pressure. The residue was purified by preparative TLC (hexane:ethyl acetate=1:10) to give the title compound as a pale yellow solid (15 mg, 25%).

후처리

  1. temperaturecooling
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customafter which the solvent was evaporated under reduced pressure
  7. customThe residue was purified by preparative TLC (hexane:ethyl acetate=1:10)

출처 및 근거

ORD 기록
ord-647e824dcc404ac691cde1adf01144e7
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822503B2

연결된 노트

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