반응 #683560

반응 방정식

8-chloro-1-(chloromethyl)-6-phenyl-4-H-s-triazolo[4,3-a][1,4]benzodiazepine

potassium iodide

methylallylamine

→

8-chloro-1-[(allylmethylamino)methyl]-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine

수율 78.7%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   기타is kept at ambient temperature
2. 2
   기타(25° C.)
3. 3
   기타for 18 hours
4. 4
   농축concentrated in vacuo
5. 5
   workup.ADDITIONThe residue is mixed with water
6. 6
   추출extracted with methylene chloride
7. 7
   세척The extract is washed with brine
8. 8
   건조dried over anhydrous sodium sulfate
9. 9
   농축concentrated
10. 10
    기타The residue is crystallized from ethyl acetate-Skellysolve B hexanes

실험 절차

A stirred mixture of 8-chloro-1-(chloromethyl)-6-phenyl-4-H-s-triazolo[4,3-a][1,4]benzodiazepine (1.37 g., 0.004 mole), potassium iodide (0.67 g., 0.004 mole), methylallylamine (0.84 g., 0.012 mole) and tetrahydrofuran (100 ml.) is kept at ambient temperature (25° C.) for 18 hours and concentrated in vacuo. The residue is mixed with water and extracted with methylene chloride. The extract is washed with brine, dried over anhydrous sodium sulfate and concentrated. The residue is crystallized from ethyl acetate-Skellysolve B hexanes to give 1.19 g of 8-chloro-1-[(allylmethylamino)methyl]-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine of melting point 157°-160° C. The analytical sample has a melting point of 158° -164° C. Anal. calcd. for C21H20ClN5 : C, 66.75; H, 5.33; Cl, 9.38; N, 18.53. Found: C, 66.87; H, 5.46; Cl, 9.42; N, 18.67. Preparation 40 8-Chloro-1-[(allylmethylamino)methyl]-6-(o-chlorophenyl)-4H-s-triazolo[4,3-a][1,4]benzodiazepine

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