تفاعل #8910
ord-d45f944e0ce54e2692d6389881056355
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.WAITthe stirring was continued for another 1 h
- 2درجة الحرارةThe solution was cooled
- 3غسيلwashed with water, brine
- 4أخرىdried
- 5تركيزconcentrated
- 6أخرىThe residue was purified on a prep TLC plate
الإجراء التجريبي
To a solution of 0.38 g of the product of Step A dissolved in 3 mL of DW, was added 0.14 mL (1.07 mmol) of 1-chloropinacolone and 0.65 g of Cs2CO3. After stirring for 2 h, another 0.05 mL (0.38 mmol) of 1-chloropinacolone was added and the stirring was continued for another 1 h. Additional 0.325 g (1 mmol) of Cs2CO3 was added and the solution was heated in a 60° C. bath for 3 h. The solution was cooled, diluted with Et2O, washed with water, brine, dried and concentrated. The residue was purified on a prep TLC plate using 20% EtOAc/hexane as eluant to afford the title compound. HPLC/MS: 424 (M+1), 426 (M+3); Rt=4.49 min.