Triethylamine → 3-((4-(4-Amino-5-chloro-2-ethoxybenzoyl)piperazin-1-yl)methyl)-N-tert-butylbenzamide

HRID 1878356노트

반응식

HRID 1878356 반응식
CCCP1(OP(CCC)(=O)OP(CCC)(=O)O1)=O.[NH2:19][C:20]1[C:28]([Cl:29])=[CH:27][C:23]([C:24]([OH:26])=O)=[C:22]([O:30][CH2:31][CH3:32])[CH:21]=1.[C:33]([NH:37][C:38](=[O:52])[C:39]1[CH:44]=[CH:43][CH:42]=[C:41]([CH2:45][N:46]2[CH2:51][CH2:50][NH:49][CH2:48][CH2:47]2)[CH:40]=1)([CH3:36])([CH3:35])[CH3:34].C(N(CC)CC)C>ClCCl>[NH2:19][C:20]1[C:28]([Cl:29])=[CH:27][C:23]([C:24]([N:49]2[CH2:48][CH2:47][N:46]([CH2:45][C:41]3[CH:40]=[C:39]([CH:44]=[CH:43][CH:42]=3)[C:38]([NH:37][C:33]([CH3:35])([CH3:36])[CH3:34])=[O:52])[CH2:51][CH2:50]2)=[O:26])=[C:22]([O:30][CH2:31][CH3:32])[CH:21]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 111923Propylphosphonic anhydrideHCID 105366584-Amino-5-chloro-2-ethoxybenzoic acidHCID 66877987N-tert-butyl-3-(piperazin-1-ylmethyl)benzamide

생성물 1

HCID 579176643-((4-(4-Amino-5-chloro-2-ethoxybenzoyl)piperazin-1-yl)methyl)-N-tert-butylbenzamide수율 95.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-Propanephosphonic acid cyclic anhydride (5.90 g, 9.2 mmol, 5.52 mL) was added dropwise to a solution of 4-ammo-5-chloro-2-ethoxy benzoic acid (1 g, 4.6 mmol), N-tert-butyl-3-(piperazin-1-ylmethyl)benzamide (1.40 g, 5.1 mmol) and triethylamine (1.401 g, 13.8 mmol, 1.93 mL) in dichloromethane. The reaction mixture was stirred at room temperature for 2 hours. The reaction was concentrated under reduced pressure and the residue was taken up in ethyl acetate, washed with water, sodium hydrogen carbonate and brine. The organic phase was concentrated under vacuum to afford the title compound (2.08 g).

후처리

  1. concentrationThe reaction was concentrated under reduced pressure
  2. washwashed with water, sodium hydrogen carbonate and brine
  3. concentrationThe organic phase was concentrated under vacuum

출처 및 근거

ORD 기록
ord-83da8fae4dfe46ea8d698f3dd0738f2f
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314091B2

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