Triethylamine → Benzene, [(2-isocyanatoethoxy)methyl]-

In 80 ml of AcOEt was dissolved 8.70 g of 3-benzyloxypropionic acid, and 6.80 ml of Et3N and 5.10 ml of ethyl chlorocarbonate were added to the solution at -10° C., and the mixture was stirred for 15 minutes. Thereafter, 16 ml of an aqueous solution containing 4.78 g of sodium azide was added to the mixture, and the resulting mixture was stirred at -5° to 0° C. for 30 minutes. The reaction mixture was washed with water and dried over anhydrous magnesium sulfate. Into a flask in which 15 ml of AcOEt had been refluxed under heating, the AcOEt solution containing the acid azide was added dropwise over 20 minutes, and the mixture was further refluxed under heating for 10 minutes. After the solvent was removed, the residue was distilled under reduced pressure (97° C./4 mmHg) to obtain the title compound.

1. additionwere added to the solution at -10° C.
2. additionwas added to the mixture
3. stirringthe resulting mixture was stirred at -5° to 0° C. for 30 minutes
4. washThe reaction mixture was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. temperatureInto a flask in which 15 ml of AcOEt had been refluxed
7. temperatureunder heating
8. additionthe AcOEt solution containing the acid azide
9. additionwas added dropwise over 20 minutes
10. temperaturethe mixture was further refluxed
11. temperatureunder heating for 10 minutes
12. customAfter the solvent was removed
13. distillationthe residue was distilled under reduced pressure (97° C./4 mmHg)

ORD-Eintrag

ord-6d9f891adb954975b8a92ae7ed656a0a

Quelldatensatz

uspto-grants-1998_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05837687