Potassium Carbonate → Methyl 2-methyl-2-phenyl-6-{4-[(4'-trifluoromethyl-biphenyl-2-carbonyl)-amino]-piperidin-1-yl}-hexanecarboxylate

HRID 1167111

反応式

HRID 1167111 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][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][CH:17]=3)=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:9])[CH2:3][CH2:2]1.Br[CH2:27][CH2:28][CH2:29][CH2:30][C:31]([CH3:43])([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[CH2:32][C:33]([O:35][CH3:36])=[O:34].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:43][C:31]([C:37]1[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=1)([CH2:30][CH2:29][CH2:28][CH2:27][N:1]1[CH2:6][CH2:5][CH:4]([NH:7][C:8]([C:10]2[C:11]([C:16]3[CH:17]=[CH:18][C:19]([C:22]([F:23])([F:24])[F:25])=[CH:20][CH:21]=3)=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:9])[CH2:3][CH2:2]1)[CH2:32][C:33]([O:35][CH3:36])=[O:34]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 9928271N-(Piperidin-4-yl)-4'-(trifluoromethyl)-biphenyl-2-carboxamideHCID 22995743Methyl 6-bromo-2-methyl-2-phenyl-hexanecarboxylate

生成物 1

HCID 22995675Methyl 2-methyl-2-phenyl-6-{4-[(4'-trifluoromethyl-biphenyl-2-carbonyl)-amino]-piperidin-1-yl}-hexanecarboxylate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

0.2 g (0.574 mmol) of 4′-trifluoromethyl-biphenyl-2-carboxylic acid-piperidin-4-yl-amide, 0.15 g (0.5 mmol) of methyl 6-bromo-2-methyl-2-phenyl-hexanecarboxylate and 0.083 g (0.6 mmol) of potassium carbonate are dissolved in 10 ml of acetonitrile. The mixture is stirred for 8 hours at 60° C. and for 14 hours at ambient temperature. Then the reaction mixture is poured onto water and extracted with ethyl acetate. The organic phase is dried over sodium sulphate and the solvent is distilled off in the rotary evaporator. After column chromatography on silica gel (eluant: dichloromethane/methanol=20:1) a highly viscous oil remains.

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
  4. distillationthe solvent is distilled off in the rotary evaporator

出典と根拠

ORDレコード
ord-6cd803da8c144149904d0fa9c1848818
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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