تفاعل #49526

ord-9c4f0767ed55424bbd3d0a16a7c5bd1c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىfollowed by purification by flash column chromatography (hexane/ethyl acetate=95/5 to 80/20 to 70/30)

الإجراء التجريبي

In a similar manner to Step. 3 of Example 16, 4-chloro-5-methyl-3-hydroxy-2-(1-methyl-1-phenylethyl)isoindolinone (400 mg, 1.27 mmol) was dissolved in THF (16 mL), and the solution was treated with TMEDA (0.33 mL, 2.2 mmol), sec-butyl lithium-hexane solution (1.01 mol/L, 2.8 mL, 2.8 mmol) and iodine (387 mg, 1.52 mmol), followed by purification by flash column chromatography (hexane/ethyl acetate=95/5 to 80/20 to 70/30) to obtain 4-chloro-5-methyl-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (352 mg, yield 63%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745641B2uspto-grants-2010_06