反应详情

A solution of 3-chloro-3-methyl-2-nitrosobutane (25.5 g) in methanol (180 cm3) was added dropwise to a stirred solution of 1,3-diaminopropane (47 cm3) in methanol (75 cm3) at 0° C. After the addition was complete the mixture was refluxed for 6 hours. Removal of the methanol in vacuo gave a yellow oil which was slurried in water (50 cm3). The white precipitate was removed by filtration and the pH of the aqueous solution adjusted to about 11. After saturating with salt the solution was continuously extracted with dichloromethane for 36 hours. The organic phase was dried (MgSO4) and concentrated in vacuo giving a yellow oil. Recrystallisation from ether/petrol gave pure product as a white crystalline solid, 9.9 g. Mpt. 69°-72° C.

1. additionAfter the addition
2. temperaturewas refluxed for 6 hours
3. customRemoval of the methanol in vacuo
4. customgave a yellow oil which
5. customThe white precipitate was removed by filtration
6. concentrationAfter saturating with salt the solution
7. extractionwas continuously extracted with dichloromethane for 36 hours
8. dry with materialThe organic phase was dried (MgSO4)
9. concentrationconcentrated in vacuo
10. customgiving a yellow oil
11. customRecrystallisation from ether/petrol
12. customgave pure product as a white crystalline solid, 9.9 g
13. custom69°-72° C.