Water → [3-(4-methoxy-phenyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-5-yl]-(1H-pyrazol-4-yl)-amine

HRID 1481250노트

반응식

HRID 1481250 반응식
Cl[C:2]1[N:3]=[CH:4][C:5]2[N:10]=[N:9][N:8]([C:11]3[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=3)[C:6]=2[N:7]=1.C(OC([N:26]1[CH:30]=[C:29]([NH2:31])[CH:28]=[N:27]1)=O)(C)(C)C.O>COCCO>[CH3:18][O:17][C:14]1[CH:15]=[CH:16][C:11]([N:8]2[C:6]3[N:7]=[C:2]([NH:31][C:29]4[CH:30]=[N:26][NH:27][CH:28]=4)[N:3]=[CH:4][C:5]=3[N:10]=[N:9]2)=[CH:12][CH:13]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 59587648tert-butyl 4-amino-1H-pyrazole-1-carboxylateHCID 897179715-Chloro-3-(4-methoxy-phenyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine

생성물 1

HCID 71666908[3-(4-methoxy-phenyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-5-yl]-(1H-pyrazol-4-yl)-amine

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

실험 절차

A solution of 262 mg (1.00 mmol) 5-chloro-3-(4-methoxy-phenyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine and 183 mg (1.00 mmol) 4-amino-pyrazole-1-carboxylic acid tert-butyl ester in 2.5 ml 2-methoxy-ethanol is stirred for 3 hours at 100° C. The reaction mixture is cooled to room temperature and water is added. The resulting precipitate is filtered off, washed with water and dried. The crude product is recrystallized from isopropanol giving “A3” as brown crystals; HPLC/MS (A): 1.6 min, [M+H] 309;

후처리

  1. filtrationThe resulting precipitate is filtered off
  2. washwashed with water
  3. customdried
  4. customThe crude product is recrystallized from isopropanol giving “A3” as brown crystals
  5. custom1.6 min, [M+H] 309

출처 및 근거

ORD 기록
ord-7660a1f517f943c4b24129788ee80fdc
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409914B2

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