تفاعل #215685

ord-84d9e50fa4d64588889b44e09408c682

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىat 0° C
  2. 2
    استخلاصThe mixture was extracted with dichloromethane several times
  3. 3
    غسيلThe combined organic layer was washed with H2O and saturated NaCl solution
  4. 4
    تجفيفdried over Na2SO4
  5. 5
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

To a solution of sodium 6β-[(1,3-dithiolan-2-ylidene)(ethoxycarbonyl)acetamido]-2,2-dimethylpenam-3-carboxylate (46 mg, 0.1 mmol) in 1 mL of H2O was added one drop (38 mg) of cone. HCl solution at 0° C. The mixture was extracted with dichloromethane several times. The combined organic layer was washed with H2O and saturated NaCl solution, dried over Na2SO4, and concentrated under reduced pressure to give the title compound (32 g, 74% yield) as a yellow oil: 1H NMR (D2O) δ 1.40 (3H, t, J=7Hz, CH2CH3), 1.55 and 1.66 (each 3H, s, C2 -(CH3)2), 3.33 (4H, s, SCH2CH2S), 4.31-4.41 (3H, m, C3 -H and OCH2CH3), 5.57 (1H, d, J=4Hz, C5-H), 5.82 (1H, dd, J=4 and 9Hz, C6-H), 9.03 (1H, d, J=9Hz, NH).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05464616uspto-grants-1995_11