تفاعل #79567

ord-e166723ebbaa4739aeb3ed3b4ce9f563

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe solvent removed under reduced pressure
  2. 2
    أخرىThe residue was partitioned between ethyl acetate and water
  3. 3
    غسيلthe organic layer washed with brine
  4. 4
    تجفيفdried over magnesium sulfate
  5. 5
    أخرىThe ethyl acetate solution was absorbed onto silica gel, which
  6. 6
    غسيلwas eluted with 10% ethyl acetate/hexane

الإجراء التجريبي

To a solution of 1,3,3-trimethylbicyclo[2.2.1]hept-2-ylamine (5 g, 26.3 mmol) in methylene chloride (20 ml) and triethylamine (4 ml) was added chloroacetyl chloride (2.1 ml, 26.4 mmol) dropwise. The resulting solution was stirred for 12 hours, then the solvent removed under reduced pressure. The residue was partitioned between ethyl acetate and water, the organic layer washed with brine, and dried over magnesium sulfate. The ethyl acetate solution was absorbed onto silica gel, which was eluted with 10% ethyl acetate/hexane, to yield 2-chloro-N-(1,3,3-trimethylbicyclo[2,2,1]hept-2-yl)acetamide as a white solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06713650B2uspto-grants-2004_03