تفاعل #949433

ord-8f56889448be44a3bbdbad46cc86450b

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwas degassed under nitrogen
  2. 2
    تركيزThe mixture was concentrated under vacuum
  3. 3
    استخلاصextracted with 2×10 ml of ether
  4. 4
    غسيلwashed successively with water and saturated NaCl solution
  5. 5
    تجفيفdried (MgSO4)
  6. 6
    أخرىThe solvent was removed in vacuo

الإجراء التجريبي

A mixture of 380 mg (1.69 mmol) of trimethylsilyl (4,4,7-trimethyl-thiochroman-6-yl) ethyne, (Compound 67) 4 ml of isopropanol and 2.5 ml of aqueous 1N potassium hydroxide was degassed under nitrogen and stirred at room temperature for 16 h. The mixture was concentrated under vacuum and extracted with 2×10 ml of ether. The ether extracts were combined and washed successively with water and saturated NaCl solution and then dried (MgSO4). The solvent was removed in vacuo to give the title compound as a yellow oil. PMR (CDCl3): & 1.31 (6H, s), 1.88-1.96 (2H, m), 2.35 (3H, s), 3.00-3.08 (2H, m), 3.25 (1H, s), 6.94 (1H, s), 7.47 (1H, s).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05717094uspto-grants-1998_02