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

HRID 1167107

反応式

HRID 1167107 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([NH:7][C:8]([C:10]2[C:11]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:9])[CH2:3][CH2:2]1.Br[CH2:23][CH2:24][CH2:25][C:26]([CH3:38])([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[CH2:27][C:28]([O:30][CH3:31])=[O:29].C(N(CC)CC)C>CN(C)C=O>[CH3:38][C:26]([C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1)([CH2:25][CH2:24][CH2:23][N:1]1[CH2:6][CH2:5][CH:4]([NH:7][C:8]([C:10]2[C:11]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:9])[CH2:3][CH2:2]1)[CH2:27][C:28]([O:30][CH3:31])=[O:29]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 113918514-[(2-Biphenyl)carbonylamino]piperidineHCID 22995606Methyl 5-bromo-2-methyl-2-phenyl-pentanecarboxylate

生成物 1

HCID 22995520Methyl 2-methyl-2-phenyl-5-{4-[(biphenyl-2-carbonyl)-amino]-piperidin-1-yl}-pentanecarboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A solution of 0.634 g (0.002 mol) of biphenyl-2-carboxylic acid-piperidin-4-ylamide, 0.5 g (1.75 mmol) of methyl 5-bromo-2-methyl-2-phenyl-pentanecarboxylate and 1 ml (0.007 mol) of triethylamine are dissolved in 3 ml dimethylformamide. The mixture is stirred for 14 hours at 80° C. Then the reaction mixture is poured onto water and extracted with ethyl acetate. The organic phase is dried over sodium sulphate. After column chromatography on silica gel (eluant: dichloromethane/methanol=10:1) colourless crystals remain.

後処理

  1. additionThen the reaction mixture is poured onto water
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phase is dried over sodium sulphate

出典と根拠

ORDレコード
ord-be0aaedc435e4e1c9fd25e02e5d8de5a
出典データセット
uspto-grants-2003_09
特許番号
US06617325B1

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