Phosphorus tribromide → HCID 86680883、化合物

Diethylether (250 ml) was added to N-(11-hydroxy-undecyl)-N-methyl acrylamide (38.31 g, 0.150 mol) and BHT (10 mg). Phosphorus tribromide (13.53 g, 50.0 mmol) was added dropwise. The initially undissolved solid dissolved completely and a yellowish oil precipitated. The reaction mixture was stirred at ambient temperature. After 24 h water (100 ml) and dichloromethane (200 ml) were added and the phases were separated. The aqueous phase was extracted with dichloromethane (2×100 ml). The combined organic phases were dried over Na2SO4, filtered, concentrated on the rotary evaporator and dried on the fine vacuum. The yellowish oil was dissolved in dichloromethane (100 ml) and filtered via a fritted-glass filter filled with diatomaceous earth (n-hexane/ethyl acetate 1:1). The eluent was concentrated on the rotary evaporator and dried under a fine vacuum. 25.25 g (79.3 mmol; 53% yield) of a yellowish oil was obtained.

1. dissolutionThe initially undissolved solid dissolved completely
2. customa yellowish oil precipitated
3. additionAfter 24 h water (100 ml) and dichloromethane (200 ml) were added
4. customthe phases were separated
5. extractionThe aqueous phase was extracted with dichloromethane (2×100 ml)
6. dry with materialThe combined organic phases were dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated on the rotary evaporator
9. customdried on the fine vacuum
10. dissolutionThe yellowish oil was dissolved in dichloromethane (100 ml)
11. filtrationfiltered via a fritted-glass
12. filtrationfilter
13. additionfilled with diatomaceous earth (n-hexane/ethyl acetate 1:1)
14. concentrationThe eluent was concentrated on the rotary evaporator
15. customdried under a fine vacuum
16. custom25.25 g (79.3 mmol; 53% yield) of a yellowish oil was obtained

ORDレコード

ord-fc4713466cb94923a7d488a3eec961bb

出典データセット

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09393181B2