反应详情

温度

50 °C

To a stirred solution of 1.2 parts of sodium hydroxide in 40 parts of methanol were added 7.8 parts of 1-hydroxy-α-phenyl-1H-benzotriazole-6-methanol. After concentration, 18 parts of methylbenzene were added to the concentrate. The solvent was evaporated again and the residue was dissolved in 27 parts of N,N-dimethylformamide. 5.52 Parts of 1-iodobutane were added at once and the whole was stirred for 30 minutes at 50° C. After concentration, 30 parts of water were added. The solidified product was filtered off, washed with water and dissolved in dichloromethane. The organic layer was dried, filtered and evaporated. The residue was crystallized from 17.5 parts of 2,2'-oxybispropane. The product was filtered off and dried, yielding 7.8 parts (87.4%) of 1-butoxy-α-phenyl-1H-benzotriazole-6-methanol; mp. 89.2° C. (int. 65).

1. concentrationAfter concentration, 18 parts of methylbenzene
2. additionwere added to the concentrate
3. customThe solvent was evaporated again
4. dissolutionthe residue was dissolved in 27 parts of N,N-dimethylformamide
5. addition5.52 Parts of 1-iodobutane were added at once and the whole
6. concentrationAfter concentration, 30 parts of water
7. additionwere added
8. filtrationThe solidified product was filtered off
9. washwashed with water
10. dissolutiondissolved in dichloromethane
11. customThe organic layer was dried
12. filtrationfiltered
13. customevaporated
14. customThe residue was crystallized from 17.5 parts of 2,2'-oxybispropane
15. filtrationThe product was filtered off
16. customdried