Methyl iodide → Methyl 2-methyl-2-phenyl-5-{4-[(4'-trifluoromethyl-biphenyl-2-carbonyl)-N-methyl-amino]-piperidin-1-yl}-pentanecarboxylate

HRID 1167109

反応式

HRID 1167109 の反応式
[H-].[Na+].[CH3:3][C:4]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([CH2:10][CH2:11][CH2:12][N:13]1[CH2:18][CH2:17][CH:16]([NH:19][C:20]([C:22]2[C:23]([C:28]3[CH:33]=[CH:32][C:31]([C:34]([F:37])([F:36])[F:35])=[CH:30][CH:29]=3)=[CH:24][CH:25]=[CH:26][CH:27]=2)=[O:21])[CH2:15][CH2:14]1)[CH2:5][C:6]([O:8][CH3:9])=[O:7].[CH3:44]I>CN(C)C=O>[CH3:3][C:4]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([CH2:10][CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][CH:16]([N:19]([C:20]([C:22]2[C:23]([C:28]3[CH:33]=[CH:32][C:31]([C:34]([F:35])([F:36])[F:37])=[CH:30][CH:29]=3)=[CH:24][CH:25]=[CH:26][CH:27]=2)=[O:21])[CH3:44])[CH2:17][CH2:18]1)[CH2:5][C:6]([O:8][CH3:9])=[O:7]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 22995529Methyl 2-methyl-2-phenyl-5-{4-[(4'-trifluoromethyl-biphenyl-2-carbonyl)-amino]-piperidin-1-yl}-pentanecarboxylate

生成物 1

HCID 22995623Methyl 2-methyl-2-phenyl-5-{4-[(4'-trifluoromethyl-biphenyl-2-carbonyl)-N-methyl-amino]-piperidin-1-yl}-pentanecarboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.095 g (0.803 mmol) of sodium hydride (55 to 65% in oil) are added to a solution of 0.4 g (0.724 mmol) of methyl 2-methyl-2-phenyl-5-{4-[(4′-trifluoromethyl-biphenyl-2-carbonyl)-amino]-piperidin-1-yl}-pentanecarboxylate in 5 ml of dimethylformamide at ambient temperature and stirred for one hour. Then 0.05 ml (0.803 mmol) of methyl iodide are added and the mixture is stirred for 14 hours. The reaction solution is poured onto water, extracted with ethyl acetate, and the organic phase is dried over sodium sulphate. The product is purified by column chromatography on silica gel (eluant: dichloromethane/methanol=5:1).

後処理

  1. stirringthe mixture is stirred for 14 hours
  2. additionThe reaction solution is poured onto water
  3. extractionextracted with ethyl acetate
  4. dry with materialthe organic phase is dried over sodium sulphate
  5. customThe product is purified by column chromatography on silica gel (eluant: dichloromethane/methanol=5:1)

出典と根拠

ORDレコード
ord-d437bc1c3c4347738e67317dc95dccbc
出典データセット
uspto-grants-2003_09
特許番号
US06617325B1

関連ノート

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