تفاعل #1179916

ord-e975758c79c64f1bac8404f5b47ef947

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled in an ice bath
  2. 2
    ترشيحThe precipitate was filtered
  3. 3
    غسيلwashed twice with ether
  4. 4
    أخرىThe filtrate was separated
  5. 5
    استخلاصthe aqueous phase was extracted with ether
  6. 6
    تجفيفThe combined ethereal solutions were dried (MgSO4)
  7. 7
    أخرىevaporated

الإجراء التجريبي

Ethyl potassium malonate (25.0 g, 0.15 mol) was suspended in water (15.6 ml) and cooled in an ice bath. Concentrated HCl (12.5 ml) was added dropwise over 30 min, then the mixture was stirred for a further 10 min. The precipitate was filtered, then washed twice with ether. The filtrate was separated and the aqueous phase was extracted with ether. The combined ethereal solutions were dried (MgSO4) and evaporated to afford, as an oil, monoethyl hydrogen malonate (19.2 g, 99%) which was dried under vacuum overnight (or 50°/1 mm for 1 h) prior to use.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08129527B2uspto-grants-2012_03