Hydrochloric Acid → 5-[(3-Chlorophenyl)methoxy]-3-(1-piperazinyl)-2-pyrazinamine

HRID 2182152ノート

反応式

HRID 2182152 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:19]([NH2:20])=[N:18][CH:17]=[C:16]([O:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([Cl:29])[CH:24]=3)[N:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>O1CCOCC1>[Cl:29][C:25]1[CH:24]=[C:23]([CH:28]=[CH:27][CH:26]=1)[CH2:22][O:21][C:16]1[N:15]=[C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)[C:19]([NH2:20])=[N:18][CH:17]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 69732063HCID 69732063、化合物

生成物 1

HCID 98367235-[(3-Chlorophenyl)methoxy]-3-(1-piperazinyl)-2-pyrazinamine収率 17%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
40 °C

実験手順

3′-Amino-6′-(3-chloro-benzyloxy)-2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-carboxylic acid tert-butyl ester I-3s (150 mg, 357 μmol) was dissolved in 1,4-dioxane (6 mL) and an HCl solution (0.90 mL, 4 M in 1,4-dioxane, 3.6 mmol) was added with stirring at 40° C. The solution was stirred at 40° C. for 18 h and concentrated in vacuo to approximately 2 mL. The mixture was diluted with Et2O. The resulting brown solid was collected by filtration and washed twice with Et2O. The solid was purified by preparative HPLC to give the title compound 3-P as a tan solid (19 mg, 17% yield).

後処理

  1. stirringThe solution was stirred at 40° C. for 18 h
  2. concentrationconcentrated in vacuo to approximately 2 mL
  3. additionThe mixture was diluted with Et2O
  4. filtrationThe resulting brown solid was collected by filtration
  5. washwashed twice with Et2O
  6. customThe solid was purified by preparative HPLC

出典と根拠

ORDレコード
ord-c812a46b5bf5470d9f8ce90c22d6b8f8
出典データセット
uspto-grants-2005_05
特許番号
US06894050B2

反応ノート

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