Dimethylamine → HCID 57469086, 화합물

HRID 1928438노트

반응식

HRID 1928438 반응식
[CH3:1][NH:2][CH3:3].C(N(CC)CC)C.Cl.[F:12][C:13]([F:47])([F:46])[C:14]1[CH:19]=[C:18]([C:20]2[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][CH:21]=2)[N:17]=[C:16]([C:30]2[CH:35]=[CH:34][N:33]=[C:32]([C:36]3[CH:37]=[C:38]([S:42](Cl)(=[O:44])=[O:43])[CH:39]=[CH:40][CH:41]=3)[CH:31]=2)[N:15]=1>C1COCC1>[CH3:1][N:2]([CH3:3])[S:42]([C:38]1[CH:39]=[CH:40][CH:41]=[C:36]([C:32]2[CH:31]=[C:30]([C:16]3[N:15]=[C:14]([C:13]([F:12])([F:46])[F:47])[CH:19]=[C:18]([C:20]4[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:27])[F:28])=[CH:22][CH:21]=4)[N:17]=3)[CH:35]=[CH:34][N:33]=2)[CH:37]=1)(=[O:43])=[O:44]

참가 물질

5

반응물 3

HCID 674DimethylamineHCID 8471TriethylamineHCID 60209344HCID 60209344, 화합물

생성물 1

HCID 57469086HCID 57469086, 화합물수율 97%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a cooled (ice-water bath) and stirred mixture of dimethylamine solution (60% in water) (0.27 ml, 3.21 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 (0.5 g, 97%). MS (ISP) 552.7 [(M+H)+]; mp 225° 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-17249edf24f14dbcaa11801a0589ec19
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183262B2

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