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Trifluoroacetic acid → HCID 86679769, 화합물

HRID 77479
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인쇄 미리보기

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HRID 77479 반응식
O1CCCCC1[N:7]1[C:15]2[C:10](=[CH:11][C:12]([CH2:16][CH2:17][C:18]3[N:23]=[CH:22][N:21]=[C:20]([NH:24][C:25]4[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[CH:27][CH:26]=4)[N:19]=3)=[CH:13][CH:14]=2)[CH:9]=[N:8]1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH:7]1[C:15]2[C:10](=[CH:11][C:12]([CH2:16][CH2:17][C:18]3[N:23]=[CH:22][N:21]=[C:20]([NH:24][C:25]4[CH:30]=[CH:29][C:28]([C:31]([F:33])([F:34])[F:32])=[CH:27][CH:26]=4)[N:19]=3)=[CH:13][CH:14]=2)[CH:9]=[N:8]1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 866797684-(2-(1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-5-yl)ethyl)-N-(4-(trifluoromethyl)phenyl)-1,3,5-triazin-2-amine

생성물 1

HCID 86679769HCID 86679769, 화합물수율 16.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
23 °C

실험 절차

To a solution of 4-(2-(1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-5-yl)ethyl)-N-(4-(trifluoromethyl)phenyl)-1,3,5-triazin-2-amine (0.03 g, 0.064 mmol) in DCM (2 mL) cooled to 0° C., TFA (0.025 mL, 0.320 mmol) was added and the reaction mixture was stirred at 23° C. overnight. The reaction mixture was concentrated, washed with diethyl ether, and purified by preparative HPLC on a SY C18 column (20×19 mm) using 0-100% mobile phase B (ACN) in mobile phase A (10 mM NH4OAc) over 17 min to give 4-(2-(1H-indazol-5-yl)ethyl)-N-(4-(trifluoromethyl)phenyl)-1,3,5-triazin-2-amine as a white solid (4 mg, 16%).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. washwashed with diethyl ether
  3. custompurified by preparative HPLC on a SY C18 column (20×19 mm)
  4. customover 17 min

출처 및 근거

ORD 기록
ord-ffe8a94bf6044f38b2450b7920966a13
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08841301B2

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