反应详情

To a solution of triflic anhydride (16.5 ml, 0.1 mol) in chloroform (50 ml) is added a solution of 2-methyl-2-nitro-1,3-propanediol (6.75 g, 0.05 mol) and pyridine (8.85 ml, 0.11 mol) in chloroform (50 ml) with external cooling to ensure a temperature of between 0° and 5° C. during the addition. After the addition the cooling bath is removed and the reaction stirred for 18 hours at ambient temperature. The reaction mixture is transferred to a separating funnel and washed with water. The organic layer is dried (Na2SO4), filtered and evaporated to dryness. The crude product is purified by chromatography using a 4:1 mixture of Hexane:Ethyl acetate as eluant; the product is obtained as a solid with melting point 50-52° C.

1. temperaturewith external cooling
2. customa temperature of between 0° and 5° C.
3. additionduring the addition
4. additionAfter the addition the cooling bath
5. customis removed
6. customThe reaction mixture is transferred to a separating funnel
7. washwashed with water
8. dry with materialThe organic layer is dried (Na2SO4)
9. filtrationfiltered
10. customevaporated to dryness
11. customThe crude product is purified by chromatography
12. additiona 4:1 mixture of Hexane
13. customthe product is obtained as a solid with melting point 50-52° C.