تفاعل #2483264

ord-b685eade98604f9f8ba3bb9586b70bbd

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

الإجراء التجريبي

To a solution of the title compound of Step B (Example 1) 0.4 g, 0.96 mmol)in 5 ml methylene chloride was added triethylamine (0.12 g) and cooled to 0° C. To this solution was added (1-methylpropoxycarbonyl)sulfenyl chloride (Step A) (0.2 g, 0.0012 mol). The mixture was stirred at room temperature for one hour. At this stage thin layer chromatography indicated only partial conversion, therefor, additional amounts of (1-methylpropoxycarbonyl)sulfenyl chloride (0.2 g) and triethylamine (0.12g) was added and the mixture was let stand over night. The reaction mixturewas subjected to silica gel column chromatography using hexane-ether (7:1) as eluent. The title compound was obtained (0 g) in high purity; m.p.: 125°-126° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05491162uspto-grants-1996_02