تفاعل #166413
ord-ab295fc97e9f47a881009d73c7510aad
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةAfter 1.25 hours of reflux the reaction
- 2أخرىquenched with water (2.22 mL)
- 3ترشيحThe remaining solids were filtered off
- 4تركيزthe filtrate was concentrated
الإجراء التجريبي
To a stirring mixture of lithium aluminum hydride (2.22 g, 58.5 mmol) in tetrahydrofuran (70 mL) was added compound 399 (3.60 g, 13.8 mmol), portionwise over three minutes. After 1.25 hours of reflux the reaction was cooled to room temperature and quenched with water (2.22 mL), then 1N NaOH (2.22 mL), then water (2×2.22 mL). The remaining solids were filtered off, and the filtrate was concentrated to give compound 402 (2.81 g, 82%). LCMS-ESI (POS), M/Z, M+1: Found 247.1, Calculated 247.2.