反应详情

To a solution of 5.13 g of m-nitro-benzyl chloride in 100 ml benzene at 10° C. was added in small portions 6.2 g of dipropylamine over a period of 15 minutes. The reaction mixture was stirred and allowed to come to room temperature for 1.5 hours, and was then refluxed for 4 hours. Water was added to the solution and the organic layer was separated and collected. The organic layer was washed with water (3×100 ml), dried (MgSO4) and stripped to leave a dark-red oil. The product (Compound No. 1) was chromatographed over silica gel (hexane: CH2Cl2 ; 1.0:0; 4:1), to yield the title product as a yellow-amber oil. Analysis: C: calculated, 66.08; found, 65.38. H: calculated, 8.53; found 8.55. N: calculated, 11.85; found, 11.73.

1. temperaturewas then refluxed for 4 hours
2. customthe organic layer was separated
3. customcollected
4. washThe organic layer was washed with water (3×100 ml)
5. dry with materialdried (MgSO4)
6. customto leave a dark-red oil
7. customThe product (Compound No. 1) was chromatographed over silica gel (hexane: CH2Cl2 ; 1.0:0; 4:1)