Sodium Hydroxide → 1-Methyl-3-amino-5-[3-(4-piperidinomethylpyrazol-1-yloxy)propylamino]-1,2,4-triazole

HRID 232023ノート

反応式

HRID 232023 の反応式
[N:1]1([CH2:7][C:8]2[CH:9]=[N:10][N:11]([O:13][CH2:14][CH2:15][CH2:16][NH2:17])[CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:18]([N:20]=[C:21]([N:24]([CH3:33])[N:25]=CC1C=CC=CC=1)SC)#[N:19].[OH-].[Na+]>Cl>[CH3:33][N:24]1[C:21]([NH:17][CH2:16][CH2:15][CH2:14][O:13][N:11]2[CH:12]=[C:8]([CH2:7][N:1]3[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)[CH:9]=[N:10]2)=[N:20][C:18]([NH2:19])=[N:25]1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 138232143-(4-Piperidinomethylpyrazol-1-yloxy)propylamineHCID 54323404methyl N-cyano-1-methyl-2-(phenylmethylene)-hydrazinecarboximidothioate

生成物 1

HCID 200308051-Methyl-3-amino-5-[3-(4-piperidinomethylpyrazol-1-yloxy)propylamino]-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
70 °C

実験手順

5 g of 3-(4-piperidinomethylpyrazol-1-yloxy)-propylamine and 4.9 g of methyl N-cyano-1-methyl-2-(phenylmethylene)-hydrazinecarboximidothioate are combined, and heated at 70° C. for 1 hour. Thereafter, the reaction mixture is taken up with 40 ml of 1N hydrochloric acid, stirred for 1 hour at room temperature, rendered alkaline with sodium hydroxide solution and extracted with methylene chloride. The residue which remains after the solvent has been expelled is chromatographed over neutral Al2O3 (activity level III), using methylene chloride/3% strength methanol as the mobile phase. The oily title compound is reacted with tartaric acid in isopropanol to give an amorphous solid.

後処理

  1. extractionextracted with methylene chloride
  2. customhas been expelled is chromatographed over neutral Al2O3 (activity level III)
  3. customThe oily title compound is reacted with tartaric acid in isopropanol
  4. customto give an amorphous solid

出典と根拠

ORDレコード
ord-138c7c0278b04dafbb97a21f50060891
出典データセット
uspto-grants-1989_07
特許番号
US04851410

反応ノート

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