Ammonium Chloride → HCID 58609719, Verbindung

According to the description in a reference (see: Syn. Lett. 07, 1053-1054, 1999), the title compound was prepared as follows. 50 g (146 mmole) of ethyl 2-{[t-butyl(diphenyl)silyl]oxy}acetate was dissolved in 700 ml of tetrahydrofuran (THF) and 30.0 ml of titaniumtetraisopropoxide was added thereto. To the mixture was slowly added 290 ml of propylmagnesiumchloride (2.0M in THF) at −10° C., and the reaction solution was stirred for 12 hours at room temperature. 200 ml of saturated ammonium chloride was added to stop the reaction. The tetrahydrofuran (THF) used as a solvent was removed by distillation under reduced pressure, and the reaction mixture was extracted twice with 2000 ml of n-hexane. The n-hexane extract was distilled under reduced pressure and purified by silica gel column to give 42 g of the title compound.

1. customthe title compound was prepared
2. customat −10° C.
3. customthe reaction
4. customwas removed by distillation under reduced pressure
5. extractionthe reaction mixture was extracted twice with 2000 ml of n-hexane
6. extractionThe n-hexane extract
7. distillationwas distilled under reduced pressure
8. custompurified by silica gel column

ORD-Eintrag

ord-108cdc1fc36143cba86e26d7d7e42b6a

Quelldatensatz

uspto-grants-2010_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07723319B2