Potassium Carbonate → HCID 86725664, 화합물

HRID 878714

반응식

HRID 878714 반응식
CS(O[CH2:6][CH2:7][C:8]1[CH:9]=[N:10][N:11]([C:13]2[CH:18]=[C:17]([C:19]#[N:20])[CH:16]=[CH:15][N:14]=2)[CH:12]=1)(=O)=O.[F:21][C:22]1[CH:30]=[CH:29][C:25]([CH2:26][NH:27][CH3:28])=[CH:24][CH:23]=1.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[F:21][C:22]1[CH:30]=[CH:29][C:25]([CH2:26][N:27]([CH3:28])[CH2:6][CH2:7][C:8]2[CH:9]=[N:10][N:11]([C:13]3[CH:18]=[C:17]([C:19]#[N:20])[CH:16]=[CH:15][N:14]=3)[CH:12]=2)=[CH:24][CH:23]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 7368601-(4-fluorophenyl)-N-methylmethanamineHCID 867256652-[1-(4-Cyanopyridin-2-yl)pyrazol-4-yl]ethyl methanesulfonate

생성물 1

HCID 86725664HCID 86725664, 화합물수율 50.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
80 °C

실험 절차

To a mixture of 2-[1-(4-cyanopyridin-2-yl)pyrazol-4-yl]ethyl methanesulfonate (476 mg, 1.6 mmol) and (4-fluoro-benzyl)-methyl-amine (444 mg, 3.2 mmol) in ACN (30 mL) at rt was added K2CO3 (4.5 g, 32 mmol) and KI (1.0 g, 6.2 mmol. The reaction mixture was heated to 80° C. and stirred overnight. Filtered, solvent removed and purified by prep-HPLC to give the title compound (270 mg, 50%). [M+H] Calc'd for C19H18FN5, 336; Found, 336.

후처리

  1. filtrationFiltered
  2. customsolvent removed
  3. custompurified by prep-HPLC

출처 및 근거

ORD 기록
ord-89e19dcb208b474e9683f7b400a39001
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987461B2

연결된 노트

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