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Dimethylformamide → N1-(3-Fluorobenzyl)-2-[1-[2-[1-(cyclopropylmethyl)-2-oxo-1,2-dihydro-3-pyridinyl]ethyl]-2-piperidyl]acetamide

HRID 1837758
ノート
印刷プレビュー

反応式

HRID 1837758 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][CH:27]=1)[CH2:5][NH:6][C:7](=[O:24])[CH2:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][N:10]1[CH2:15][CH2:16][C:17]1[C:18](=[O:23])[NH:19][CH:20]=[CH:21][CH:22]=1.[CH:28]1([CH2:31]Cl)[CH2:30][CH2:29]1.C(=O)([O-])[O-].[K+].[K+].CN(C=O)C>O>[F:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][CH:27]=1)[CH2:5][NH:6][C:7](=[O:24])[CH2:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][N:10]1[CH2:15][CH2:16][C:17]1[C:18](=[O:23])[N:19]([CH2:31][CH:28]2[CH2:30][CH2:29]2)[CH:20]=[CH:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 80013(Chloromethyl)cyclopropaneHCID 22678298N1-(3-Fluorobenzyl)-2-[1-[2-(2-oxo-1,2-dihydro-3-pyridinyl)ethyl]-2-piperidyl]acetamide

生成物 1

HCID 22678543N1-(3-Fluorobenzyl)-2-[1-[2-[1-(cyclopropylmethyl)-2-oxo-1,2-dihydro-3-pyridinyl]ethyl]-2-piperidyl]acetamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

230 mg of N1-(3-fluorobenzyl)-2-[1-[2-(2-oxo-1,2-dihydro-3-pyridinyl)ethyl]-2-piperidyl]acetamide obtained in Example 198, 0.08 ml of cyclopropylmethyl chloride, 450 mg of potassium carbonate and 5 ml of DMF were stirred at 60° C. for 1 hour. Water was added thereto, and the mixture was extracted with ethyl acetate. The extract was dried over sodium sulfate. The drying agent was filtered off, and the solvent was evaporated. The residue was purified by NH-silica gel column chromatography (hexane:ethyl acetate=1:1, subsequently ethyl acetate), to give 180 mg of a colorless oil.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe extract was dried over sodium sulfate
  3. filtrationThe drying agent was filtered off
  4. customthe solvent was evaporated
  5. customThe residue was purified by NH-silica gel column chromatography (hexane

出典と根拠

ORDレコード
ord-67a8a4aa8c98467b876e4634ec38b19c
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06784192B2

反応ノート

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