Реакция #8896

ord-9b9d55aab8b243c5a6fc73781db5ccd2

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Промывкаwashed two times with aqueous sodium bicarbonate
  2. 2
    СушкаThe organic layer was dried over sodium sulfate
  3. 3
    Концентрированиеthen concentrated
  4. 4
    ДругоеThe residue was triturated in 10 mL of methanol
  5. 5
    ДругоеThe solid product was collected
  6. 6
    Промывкаrinsed two times with methanol
  7. 7
    Другоеthen dried in vacuo

Методика

The product of Step B (0.120 g; 0.253 mmol) and acetoxyacetyl chloride (0.11 mL; 1.01 mmol) were added to 2 mL of acetonitrile and stirred at room temperature. After 50 minutes the reaction mixture was diluted with ethyl acetate and washed two times with aqueous sodium bicarbonate. The organic layer was dried over sodium sulfate then concentrated. The residue was triturated in 10 mL of methanol. The solid product was collected and rinsed two times with methanol then dried in vacuo. HPLC/MS 576.8 (M+2); Rt=4.32 min.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07091216B2uspto-grants-2006_08