Water → HCID 22678292, 화합물

HRID 1837727노트

반응식

HRID 1837727 반응식
Cl.[CH3:2][S:3]([C:6]1[CH:10]=[CH:9][S:8][C:7]=1[CH2:11][CH2:12][CH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1)(=[O:5])=[O:4].Cl[CH2:20][C:21]1[C:22]([O:27][CH3:28])=[N:23][CH:24]=[CH:25][CH:26]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:28][O:27][C:22]1[C:21]([CH2:20][N:16]2[CH2:17][CH2:18][CH:13]([CH2:12][CH2:11][C:7]3[S:8][CH:9]=[CH:10][C:6]=3[S:3]([CH3:2])(=[O:4])=[O:5])[CH2:14][CH2:15]2)=[CH:26][CH:25]=[CH:24][N:23]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 149329453-(Chloromethyl)-2-methoxypyridineHCID 22678561HCID 22678561, 화합물

생성물 1

HCID 22678292HCID 22678292, 화합물수율 14.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4.41 g of 4-[2-(3-methylsulfonyl-2-thienyl)ethyl]piperidine hydrochloride, 2.36 g of 3-(chloromethyl)-2-methoxypyridine and 5.90 g of potassium carbonate were suspended in 30 ml of N,N-dimethylformamide, and the mixture was stirred for 12 hours at room temperature. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified by silica gel column chromatography (ethyl acetate:hexane=1:3), to give 809 mg of the title compound as a colorless oil (quantitatively).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated
  5. customthe crude product was purified by silica gel column chromatography (ethyl acetate:hexane=1:3)

출처 및 근거

ORD 기록
ord-a33426b64d964d0186404b13621c2708
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06784192B2

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