تفاعل #303529

ord-4fff63dded7a4491b66d734075eba79b

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىfor 15 minutes
  2. 2
    درجة الحرارةthe reaction mixture was cooled
  3. 3
    غسيلThe ethereal layer was washed with 1 N aqueous sodium hydroxide and brine
  4. 4
    تجفيفdried (magnesium sulfate)
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated in vacuo

الإجراء التجريبي

2-Methyl-2-butanol (480 mL, 4.4 mol) and vinylidene chloride (508 mL, 5.2 mol) were added to sulfuric acid (2 L) at 10° C. Methanol (1750 mL) was added slowly, and the reaction mixture reached 60 C for 15 minutes due to exotherm. After 30 min, the reaction mixture was cooled and poured into a stirred mixture of ether and ice water. The ethereal layer was washed with 1 N aqueous sodium hydroxide and brine, dried (magnesium sulfate), filtered, and concentrated in vacuo to afford methyl 3,3-dimethylpentanoate which was used in the subsequent step without further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08193228B2uspto-grants-2012_06