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Water → HCID 18072498, 화합물

HRID 552138
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HRID 552138 반응식
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:9]=[CH:8][CH:7]=[CH:6][C:4]=1[NH2:5].[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][CH:22]([C:25](Cl)=[O:26])[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].C(N(CC)CC)C.O>ClCCl>[F:1][C:2]([F:10])([F:11])[C:3]1[CH:9]=[CH:8][CH:7]=[CH:6][C:4]=1[NH:5][C:25]([CH:22]1[CH2:23][CH2:24][NH:19][CH2:20][CH2:21]1)=[O:26].[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][CH:22]([C:25](=[O:26])[NH:5][C:4]2[CH:6]=[CH:7][CH:8]=[CH:9][C:3]=2[C:2]([F:10])([F:11])[F:1])[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13]
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참가 물질

7

반응물 4

HCID 962WaterHCID 69222-(Trifluoromethyl)anilineHCID 8471TriethylamineHCID 21906247tert-Butyl 4-(Chlorocarbonyl)piperidine-1-carboxylate

생성물 2

HCID 18072498HCID 18072498, 화합물HCID 67172280HCID 67172280, 화합물

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To a stirred solution of 2-(trifluoromethyl)aniline (0.5 mL, 4.20 mmol) in dichloromethane (10.0 mL) was added 4-chlorocarbonylpiperidine-1-carboxylic acid tert-butyl ester (1.000 g, 4.00 mmol). The reaction mixture was stirred at ambient temperature for 10 minutes, then followed by the addition of triethylamine (0.6 mL, 4.20 mmol). The reaction mixture was stirred at ambient temperature for another 10 minutes. Water (5.0 mL) was added to the mixture and the organic phase separated and washed with saturated NaCl (10 mL), dried over MgSO4 and then concentrated in vacuo. The obtained crude product was purified by column chromatography to yield the desired product, 4-(2-trifluoromethylphenylcarbamoyl)piperidine-1-carboxylic acid tert-butyl ester, in 30% yield (0.450 g). 1H NMR (300 MHz, CDCl3) δ 7.97 (d, J=8.0 Hz, 1H), 7.61 (s. 1H), 7.53 (d, J=7.9 Hz, 1H), 7.47 (t, J=7.5 Hz, 1H), 7.18 (t, J=7.6 Hz, 1H), 4.13-4.04 (m, 2H), 2.77-2.69 (m, 2H), 2.44-2.34 (m, 1H), 1.87-1.93 (m, 2H), 1.70-1.57 (m, 2H), 1.40 (s. 9H). MS (ES−) m/z 371 (M−1).

후처리

  1. stirringThe reaction mixture was stirred at ambient temperature for another 10 minutes
  2. customthe organic phase separated
  3. washwashed with saturated NaCl (10 mL)
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe obtained crude product
  7. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-ff6c4261fef64993ba2e187e5e37bb15
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07951805B2

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