تفاعل #51866

ord-603affca2e4842b7b2bec7915cb213f2

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزconcentrated sulfuric as a catalyst
  2. 2
    أخرىthe volatile fractions removed in vacuo
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in ethyl ether (50 cm3)
  4. 4
    غسيلwashed with water (25 cm3)
  5. 5
    غسيلwashed with saturated sodium bicarbonate (25 cm3)
  6. 6
    غسيلwashed with brine (25 cm3)
  7. 7
    تجفيفdried over magnesium sulfate, vacuum
  8. 8
    ترشيحfiltered
  9. 9
    أخرىthe filtrate volatile fractions removed in vacuo

الإجراء التجريبي

To a solution of commercially available (3,4-dichloro-phenoxy)-acetic acid (2.65 g, 12.0 mmol) in allyl alcohol (12.0 cm3, 180 mmol) at ambient temperature under an atmosphere of dry nitrogen was added 4 drops concentrated sulfuric as a catalyst. The solution was stirred at ambient temperature for 20 hours and the volatile fractions removed in vacuo. The residue was dissolved in ethyl ether (50 cm3), washed with water (25 cm3), washed with saturated sodium bicarbonate (25 cm3), washed with brine (25 cm3), dried over magnesium sulfate, vacuum filtered and the filtrate volatile fractions removed in vacuo to afford the title compound as a colorless viscous oil (3.02 g, 96.8%) with positive ion ESI (M+H)+261.3.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06852713B2uspto-grants-2005_02