Chloro(diphenyl)silane → 2-Benzyl-1,2,3,3a,7,7a-hexahydro-4-thia-2-aza-cyclopenta[alpha]pentalene

Temperatur

60 °C

Indiumtrichloride (973 mg, 4.40 mmol) and chlorodiphenylsilane (2888 mg, 13.20 mmol) were added to a solution of the product from step f) (1192 mg, 4.40 mmol) in 20 mL of dichloroethane. The reaction mixture was heated at 60° C. overnight and then was cooled to room temperature and quenched with saturated NaHCO3 (50 ml). The reaction mixture was extracted with ethylacetate (2×50 mL). The combined organic extracts were washed with brine (50 ml), dried with MgSO4 and solvent evaporated in vacuo to afford the subtitle compound (638 mg, yield: 57%) that was used without further purification. MS calculated C16H17NS+H: 256, observed: 256.

1. temperaturewas cooled to room temperature
2. customquenched with saturated NaHCO3 (50 ml)
3. extractionThe reaction mixture was extracted with ethylacetate (2×50 mL)
4. washThe combined organic extracts were washed with brine (50 ml)
5. dry with materialdried with MgSO4 and solvent
6. customevaporated in vacuo

ORD-Eintrag

ord-e1aa197d0bd24dc7b74e830b3a5cd79a

Quelldatensatz

uspto-grants-2008_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07423056B2