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Triethylamine → HCID 57469089, 화합물

HRID 1928441
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HRID 1928441 반응식
[CH3:1][NH:2][CH2:3][CH2:4][CH3:5].C(N(CC)CC)C.Cl.[F:14][C:15]([F:49])([F:48])[C:16]1[CH:21]=[C:20]([C:22]2[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=2)[N:19]=[C:18]([C:32]2[CH:37]=[CH:36][N:35]=[C:34]([C:38]3[CH:39]=[C:40]([S:44](Cl)(=[O:46])=[O:45])[CH:41]=[CH:42][CH:43]=3)[CH:33]=2)[N:17]=1>C1COCC1>[CH3:1][N:2]([CH2:3][CH2:4][CH3:5])[S:44]([C:40]1[CH:41]=[CH:42][CH:43]=[C:38]([C:34]2[CH:33]=[C:32]([C:18]3[N:17]=[C:16]([C:15]([F:14])([F:48])[F:49])[CH:21]=[C:20]([C:22]4[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:29])[F:30])=[CH:24][CH:23]=4)[N:19]=3)[CH:37]=[CH:36][N:35]=2)[CH:39]=1)(=[O:45])=[O:46]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12315N-MethylpropylamineHCID 60209344HCID 60209344, 화합물

생성물 1

HCID 57469089HCID 57469089, 화합물수율 86%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a cooled (ice-water bath) and stirred mixture of N-methylpropylamine (0.23 g, 3.0 mmol), triethylamine (0.29 ml, 2.1 mmol) and THF (4 ml) was added drop wise a solution of 3-{4-[4-trifluoromethyl-6-(4-trifluoromethyl-phenyl)-pyrimidin-2-yl]-pyridin-2-yl}-benzenesulfonyl chloride hydrochloride (example I.1) (0.58 g, 1.0 mmol) in THF (6 ml). The mixture was allowed to stir at room temperature for 16 h. Purification of the reaction mixture by flash chromatography on silica gel (ethyl acetate/heptane) and crystallization (dichloromethane/MeOH/hexane) yielded the title compound as a white solid (0.47 g, 86%). MS (ISP) 580.6 [(M+H)+]; mp 144° C.

후처리

  1. stirringto stir at room temperature for 16 h
  2. customPurification of the reaction mixture by flash chromatography
  3. customon silica gel (ethyl acetate/heptane) and crystallization (dichloromethane/MeOH/hexane)

출처 및 근거

ORD 기록
ord-4d8c057b17b0409fa8ba61b35eb652c2
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183262B2

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