Trifluoroacetic acid → 4-methyl-N-(3-morpholinophenyl)-3-(3-pyrrolidin-3-yloxybenzamido)benzamide

HRID 502044ノート

反応式

HRID 502044 の反応式
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:19][CH2:18][CH:17]([O:20][C:21]2[CH:22]=[C:23]([CH:49]=[CH:50][CH:51]=2)[C:24]([NH:26][C:27]2[CH:28]=[C:29]([CH:45]=[CH:46][C:47]=2[CH3:48])[C:30]([NH:32][C:33]2[CH:38]=[CH:37][CH:36]=[C:35]([N:39]3[CH2:44][CH2:43][O:42][CH2:41][CH2:40]3)[CH:34]=2)=[O:31])=[O:25])[CH2:16]1)=O)(C)(C)C>C(Cl)Cl>[CH3:48][C:47]1[CH:46]=[CH:45][C:29]([C:30]([NH:32][C:33]2[CH:38]=[CH:37][CH:36]=[C:35]([N:39]3[CH2:40][CH2:41][O:42][CH2:43][CH2:44]3)[CH:34]=2)=[O:31])=[CH:28][C:27]=1[NH:26][C:24](=[O:25])[C:23]1[CH:49]=[CH:50][CH:51]=[C:21]([O:20][CH:17]2[CH2:18][CH2:19][NH:15][CH2:16]2)[CH:22]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 226361163-[3-(1-tert-butoxycarbonylpyrrolidin-3-yloxy)benzamido]-4-methyl-N-(3-morpholinophenyl)benzamide

生成物 1

HCID 226361154-methyl-N-(3-morpholinophenyl)-3-(3-pyrrolidin-3-yloxybenzamido)benzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

Trifluoroacetic acid (0.6 ml) was added to a stirred solution of 3-[3-(1-tert-butoxycarbonylpyrrolidin-3-yloxy)benzamido]-4-methyl-N-(3-morpholinophenyl)benzamide (0.3 g) in methylene chloride (6 ml) which had been cooled to 0° C. The reaction mixture was stirred at ambient temperature for 3 hours. The mixture was evaporated and the residue was triturated under diethyl ether to give the title compound, as its trifluoroacetate salt. The solid so obtained was dissolved in water (15 ml) and basified by the addition of potassium carbonate. The resultant precipitate was collected, washed with water and dried under vacuum to give the title compound (0.18 g); NMR Spectrum: (DMSOd6) 1.76 (m, 1H), 2.02 (m, 1H), 2.23 (s, 3H), 2.83 (m, 2H), 3.06 (m, 5H), 3.55 (m, 1H), 3.76 (t, 4H), 4.98 (m, 1H), 6.62 (d, 1H), 7.12 (m, 2H), 7.31 (d, 1H), 7.4 (m, 3H), 7.52 (m, 2H), 7.78 (d,. 1H), 7.99 (s, 1H), 10.07 (s, 1H), 10.08 (s, 1H); Mass Spectrum: M+H+ 501.

後処理

  1. customThe mixture was evaporated
  2. customthe residue was triturated under diethyl ether

出典と根拠

ORDレコード
ord-272c0f658b724d36a3261b0e92a4c59f
出典データセット
uspto-grants-2010_08
特許番号
US07772432B2

反応ノート

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