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

HRID 1481250ノート

反応式

HRID 1481250 の反応式
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

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

実験手順

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;

後処理

  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

出典と根拠

ORDレコード
ord-7660a1f517f943c4b24129788ee80fdc
出典データセット
uspto-grants-2016_08
特許番号
US09409914B2

反応ノート

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