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Triethylamine → N-[3-(3,5-bis(trifluoromethyl)benzyloxy)-2-phenylpropyl]-1-methylpiperidine-4-carboxamide

HRID 548199
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HRID 548199 반응식
C[C:2]1([C:8]([OH:10])=O)[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.Cl.[F:12][C:13]([F:37])([F:36])[C:14]1[CH:15]=[C:16]([CH:29]=[C:30]([C:32]([F:35])([F:34])[F:33])[CH:31]=1)[CH2:17][O:18][CH2:19][CH:20]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH2:21][NH2:22].[CH2:38](N(CC)CC)C.CCN=C=NCCCN(C)C.Cl>C(Cl)Cl.O>[F:12][C:13]([F:36])([F:37])[C:14]1[CH:15]=[C:16]([CH:29]=[C:30]([C:32]([F:34])([F:33])[F:35])[CH:31]=1)[CH2:17][O:18][CH2:19][CH:20]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH2:21][NH:22][C:8]([CH:2]1[CH2:3][CH2:4][N:5]([CH3:38])[CH2:6][CH2:7]1)=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 221045794-Methylpiperidine-4-carboxylic acidHCID 866240403-(3,5-Bis(trifluoromethyl)benzyloxy)-2-phenylpropylamine hydrochloride

생성물 1

HCID 86624039N-[3-(3,5-bis(trifluoromethyl)benzyloxy)-2-phenylpropyl]-1-methylpiperidine-4-carboxamide
수율 93%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

4-Methylpiperidine-4-carboxylic acid (0.41 g, 2.9 mmol), the compound produced in Example 17 (0.99 g, 2.9 mmol) and triethylamine (0.40 mL, 2.9 mmol) were dissolved in CH2Cl2 (10 mL) and WSC.HCl (0.56 g, 2.9 mmol) was added thereto at room temperature. After the mixture was stirred for 20 hours at room temperature, water was added to the residue obtained by evaporation of the solvent in vacuo and the mixture was extracted with ethyl acetate. The organic layers were combined, washed with water and a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was evaporated therefrom in vacuo to give Compound 1 (1.12 g, 93%) as an oily product.

후처리

  1. customat room temperature
  2. customobtained by evaporation of the solvent in vacuo
  3. extractionthe mixture was extracted with ethyl acetate
  4. washwashed with water
  5. dry with materiala saturated saline solution and dried over anhydrous sodium sulfate
  6. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-46867278d280445aa02087d1d2a66153
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07939552B2

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