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Triethylamine → 4-amino-N-[3-(3,5-bis(trifluoromethyl)benzyloxy)-2-ph enylpropyl]benzamide hydrochloride

HRID 548205
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HRID 548205 반응식
[ClH:1].[F:2][C:3]([F:27])([F:26])[C:4]1[CH:5]=[C:6]([CH:19]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:21]=1)[CH2:7][O:8][CH2:9][CH:10]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:11][NH2:12].[CH2:28](N(CC)CC)[CH3:29].CCN=C=N[CH2:40][CH2:41][CH2:42][N:43](C)C.Cl.Cl.[O:48]1[CH2:53][CH2:52]OCC1>O1CCOCC1.C(Cl)Cl>[ClH:1].[NH2:43][C:42]1[CH:41]=[CH:40][C:52]([C:53]([NH:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:9][O:8][CH2:7][C:6]2[CH:5]=[C:4]([C:3]([F:26])([F:27])[F:2])[CH:21]=[C:20]([C:22]([F:24])([F:23])[F:25])[CH:19]=2)=[O:48])=[CH:29][CH:28]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 204431481,4-Dioxane hydrochlorideHCID 866240403-(3,5-Bis(trifluoromethyl)benzyloxy)-2-phenylpropylamine hydrochloride

생성물 1

HCID 866240544-amino-N-[3-(3,5-bis(trifluoromethyl)benzyloxy)-2-ph enylpropyl]benzamide hydrochloride수율 65%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

실험 절차

Compound 67 (1.10 g, 923%) was produced as an oily product from 4-tert-butoxycarbonylaminobenzoic acid (0.57 g, 2.4 mmol), the compound produced in Example 17 (0.83 g, 2.0 mmol), triethylamine (0.28 mL, 2.0 mmol), WSC.HCl (0.46 g, 2.4 mmol) and CH2Cl2 (10 mL) according to the same manner as in Example 30. After that, Compound 67 (0.95 g, 1.6 mmol) was dissolved in dioxane (2.4 mL), 4 mol/L hydrogen chloride/dioxane (2.4 mL) was added thereto and the mixture was stirred for 20 hours at room temperature. The crystals produced after evaporation of the solvent therefrom in vacuo were filtered from petroleum ether to give Compound 61 (0.55 g, 65%).

후처리

  1. customThe crystals produced
  2. customafter evaporation of the solvent
  3. filtrationin vacuo were filtered from petroleum ether

출처 및 근거

ORD 기록
ord-0c031bac82e947dd84918c547fca1f50
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07939552B2

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