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

HRID 2415717노트

반응식

HRID 2415717 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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 (ml, 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.

후처리

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

출처 및 근거

ORD 기록
ord-cc751faaf3a2466295121e5d8fc724e7
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06821965B1

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