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

HRID 232023노트

반응식

HRID 232023 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-138c7c0278b04dafbb97a21f50060891
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851410

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