4-Chloro-2-(methylthio)pyrazolo[1,5-a][1,3,5]triazine → 4-(4-Imidazolylethylamino)-2-methylthiopyrazolo(1,5-a)-1,3,5-Triazine

HRID 1285120노트

반응식

HRID 1285120 반응식
Cl[C:2]1[N:7]2[N:8]=[CH:9][CH:10]=[C:6]2[N:5]=[C:4]([S:11][CH3:12])[N:3]=1.[NH2:13][CH2:14][CH2:15][C:16]1[N:20]=[CH:19][NH:18][CH:17]=1>CO>[NH:18]1[CH:17]=[C:16]([CH2:15][CH2:14][NH:13][C:2]2[N:7]3[N:8]=[CH:9][CH:10]=[C:6]3[N:5]=[C:4]([S:11][CH3:12])[N:3]=2)[N:20]=[CH:19]1

참가 물질

4

반응물 2

HCID 129161154-Chloro-2-(methylthio)pyrazolo[1,5-a][1,3,5]triazineHCID 178419017HCID 178419017, 화합물

생성물 1

HCID 1785034954-(4-Imidazolylethylamino)-2-methylthiopyrazolo(1,5-a)-1,3,5-Triazine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 30 mg 4-chloro-2-methylthiopyrazolo(1,5-a)-1,3,5-triazine and 33 mg free histamine in 3 ml of methanol is stirred at room temperature overnight. After evaporation of solvent, the residue is dissolved in ethylacetate, washed with water, and dried over MgSO4. After removal of solvent, the residue is subject to silica gel preparative thin layer chromatography using CHCl3 /methanol=9:1 as a developing solvent. Appropriate fractions are isolated, extracted with CHCl3 /CH3OH (3:1), and solvent removed in vacuo to dryness. 20 mg of a white solid are recovered. TLC (silica gel CHCl3 /CH3OH=3:1) Rf=0.15.

후처리

  1. customAfter evaporation of solvent
  2. dissolutionthe residue is dissolved in ethylacetate
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. customAfter removal of solvent
  6. customAppropriate fractions are isolated
  7. extractionextracted with CHCl3 /CH3OH (3:1), and solvent
  8. customremoved in vacuo to dryness
  9. custom20 mg of a white solid are recovered

출처 및 근거

ORD 기록
ord-34e9b56370cd4382b2ea2e2b55da1fa9
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04565815

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