تفاعل #160625

ord-abd59a1811df4d0583a52acc315953f7

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىis consumed
  2. 2
    تركيزThe reaction mixture was concentrated
  3. 3
    workup.ADDITIONdiluted with ethyl acetate
  4. 4
    غسيلwashed with 1M HCl
  5. 5
    تجفيفThe organic layer was dried over Na2SO4
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated
  8. 8
    أخرىpurified by flash chromatography on a silica gel column (hex:ethyl acetate 2:1)

الإجراء التجريبي

The stirred solution of 2-(3-Hydroxy-4-methoxyphenyl)acetic acid (9.82 g, 53.90 mmol) and p-Toluenesulfonic acid monohydrate (1.15 g, 6.0 mmol) in abs ethanol (100 ml) was refluxed for 4 hours or until all the starting material is consumed. The reaction mixture was concentrated, diluted with ethyl acetate and washed with 1M HCl. The organic layer was dried over Na2SO4, filtered, concentrated, and purified by flash chromatography on a silica gel column (hex:ethyl acetate 2:1) to give the title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08829058B2uspto-grants-2014_09