Water → HCID 22678292、化合物

HRID 1837727ノート

反応式

HRID 1837727 の反応式
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

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 149329453-(Chloromethyl)-2-methoxypyridineHCID 22678561HCID 22678561、化合物

生成物 1

HCID 22678292HCID 22678292、化合物収率 14.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a33426b64d964d0186404b13621c2708
出典データセット
uspto-grants-2004_08
特許番号
US06784192B2

反応ノート

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