Sodium Bicarbonate → HCID 18457684、化合物

温度

-78 °C

To a solution of O-protected pyridine dimethylcarbinol (3.0 g, 10.6 mmol) in THF (50 mL) at −78° C. was added n-BuLi 2.5 N in hexanes (4.7 ml, 11.7 mmol) followed, 1 min later, by phenylthionochloroformate (2.76 g, 16.0 mmol). The reaction was stirred at −78° C. for 40 min, then allowed to warm to RT and stirred 4 h. The final mixture was treated with saturated NaHCO3, extracted with DCM and AcOEt and combined organic layers were dried over Na2SO4 and concentrated. Purification of the residue by flash chromatography over silica gel (eluting hexane to DCM) afforded 1.5 g of O-protected pyridine propene as well as 1.8 g of starting O-protected pyridine dimethylcarbinol.

1. temperatureto warm to RT
2. stirringstirred 4 h
3. extractionextracted with DCM and AcOEt
4. dry with materialwere dried over Na2SO4
5. concentrationconcentrated
6. customPurification of the residue by flash chromatography over silica gel (eluting hexane to DCM)

ORDレコード

ord-ba061b4298194c7ebd7e904c726a84b3

出典データセット

uspto-grants-2007_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07208602B2