تفاعل #354957

ord-56f0c84f35e14713973e39e6bb314ea6

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture is refluxed for 3 hours
  2. 2
    درجة الحرارةcooled
  3. 3
    workup.ADDITIONdiluted with 400 mls
  4. 4
    استخلاصextracted with ether
  5. 5
    غسيلThe combined ethereal solutions are washed with water
  6. 6
    تجفيفdried over anhydrous sodium sulfate
  7. 7
    أخرىevaporated

الإجراء التجريبي

3-Acetoxy-3-(N-acetylisopropylaminomethyl)-7-methanesulfonamido-3,4-dihydro-2H-1,5-benzodioxepin (4.2 g., 10 millimole) in 20 ml. methanol is treated with 2 g. (50 millimoles) of sodium hydroxide in 20 ml. of methanol. The mixture is refluxed for 3 hours, cooled, and diluted with 400 mls. of water, neutralized with acid and extracted with ether. The combined ethereal solutions are washed with water, dried over anhydrous sodium sulfate, and evaporated to give 3-hydroxy-3-isopropylaminomethyl-7-methanesulfonamido-3,4-dihydro-2H-1,5-benzodioxepin.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US03944560uspto-grants-1976_03