反应 #1687668

ord-ba116b91729043b9a898dcb51a79fdc0

反应方程式

O=C(OCc1ccccc1)c1ccc(O)cc1O
benzyl 2,4-dihydroxybenzoate
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC=CCCl
methyallyl chloride
C=C(C)COc1ccc(C(=O)OCc2ccccc2)c(O)c1
benzyl 2-hydroxy-4-(2-methylallyloxy)benzoate
收率 57.5%

溶剂

反应条件

温度
40°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他brought to 70° C.
  2. 2
    过滤the salts are filtered off
  3. 3
    洗涤The salts were washed with DMF
  4. 4
    其他the solvent was evaporated off
  5. 5
    其他A brown oil was obtained which
  6. 6
    其他was purified on silica (eluent: 70/30 heptane/CH2Cl2)

实验过程

To a mixture of 17 g of benzyl 2,4-dihydroxybenzoate (0.07 mol) and 10 g of potassium carbonate (0.077 mol) in 60 ml of DMF brought to 70° C. were added 6.81 ml of methyallyl chloride (0.07 mol) dropwise over 1 hour. The mixture was left at 70° C. for 2 hours. It is cooled to about 40° C. and the salts are filtered off. The salts were washed with DMF. The liquids were combined, and the solvent was evaporated off. A brown oil was obtained which was purified on silica (eluent: 70/30 heptane/CH2Cl2). The head fractions were pooled to give 12 g (yield: 57%) of benzyl 2-hydroxy-4-(2-methylallyloxy)benzoate in the form of a colourless oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05976558uspto-grants-1999_11