تفاعل #595414

ord-c6e0f4394fac4981baacb36d8a198c26

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwashed with 1M HCl and brine
  2. 2
    تجفيفThe organic layer was dried with MgSO4
  3. 3
    تركيزconcentrated
  4. 4
    أخرىto give crude product
  5. 5
    أخرىIt was further purified by silica gel chromatography

الإجراء التجريبي

To a solution of the product of Step 3 (185.7 mg, 1.0 mmol, 1 equiv) in 1,4-dioxane (3.3 mL) was added KOH powder (67.3 mg, 1.2 mmol, 1.2 equiv). The mixture was stirred at room temperature for 24 hours. The mixture was diluted with EtOAc and washed with 1M HCl and brine. The organic layer was dried with MgSO4 and concentrated to give crude product. It was further purified by silica gel chromatography using 20% EtOAc/Hex to afford 141.8 mg colorless oil as product, yield 95.0%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09095572B2uspto-grants-2015_08