HRID26462

反应详情

EQUATION

反应方程式

HRID 26462 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.05 g of sodium and 8 ml of 3-hydroxymethylpyridine was heated at 65°-70° C. for 10 hours. To this mixture was added 2.1 g of p-isobutylphenylacetic acid methyl ester, and the whole was heated at 95°-100° C. for 8 hours. After the reaction was complete, 100 ml of water was added. The resulting mixture was extracted with ether, and the ether layer separated was dehydrated and concentrated to leave an oily residue. This residue was distilled under reduced pressure to give 1.9 g of p-isobutylphenylacetic acid-3-pyridylmethyl ester as a colorless liquid, boiling at 142°-145° C./1 mmHg. Analysis-Calculated for C18H21NO2 : C, 76.29; H, 7.47; N, 4.94. Found: C, 76.02; H, 7.38; N, 4.79. Mass spectrum: parent ion 283 m/e.

WORKUP

后处理

  1. temperaturewas heated at 65°-70° C. for 10 hours
  2. temperaturethe whole was heated at 95°-100° C. for 8 hours
  3. extractionThe resulting mixture was extracted with ether
  4. customthe ether layer separated
  5. concentrationconcentrated
  6. customto leave an oily residue
  7. distillationThis residue was distilled under reduced pressure