تفاعل #360945

ord-ffcad41a690c46caa4d9835e094ac018

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was cooled
  2. 2
    استخلاصThe mixture was extracted with 3×35 mL of ethyl acetate
  3. 3
    تجفيفthe organic layer was dried with magnesium sulfate
  4. 4
    ترشيحfiltered
  5. 5
    تركيزconcentrated in vacuo

الإجراء التجريبي

A solution of 0.87 g (2.6 mmole) of diethyl-2-(SR)-phenyl-3-(SR)-hydroxy-(SR)-cyclohexylmalonate in 12 mL of THF and 7 mL of water was treated with 3.1 mL (7.8 mmole) of 10% aqueous sodium hydroxide and the mixture was heated in an oil bath at 70° C. under nitrogen for 24 hr. The mixture was cooled, 10 mL of water was added and the pH was adjusted to 2 with 2N aqueous HCl. The mixture was extracted with 3×35 mL of ethyl acetate, and the organic layer was dried with magnesium sulfate, filtered and concentrated in vacuo to give 700 mg of a light yellow foam. This material was carried on in Step F below.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05387595uspto-grants-1995_02