HRID426728

反应详情

EQUATION

反应方程式

HRID 426728 的结构方程式

PROCEDURE

实验过程

5-amino-3-isopropyl-1-methyl pyrazole (described in British Pat. No. 1,057,740) (19.3 g) was dissolved in 180 ml. phosphorus oxychloride (POCl3). 1-Acetyl-2-imidazolidinone (J. Chem Soc 1964, 178) (20.1 g) was added. This reaction mixture was stirred at 55° for 40 hr. The solvents were concentrated in vacuum, ice and methylene chloride were added and the mixture neutralized with 25% sodium hydroxide in water. The methylene chloride layer was dried over MgSO4 and then concentrated and the residue crystallized from isopropyl alcohol and ether to give 12.73 g. of product, mp 145°-147° C.

WORKUP

后处理

  1. dissolution1,057,740) (19.3 g) was dissolved in 180 ml
  2. concentrationThe solvents were concentrated in vacuum, ice and methylene chloride
  3. additionwere added
  4. dry with materialThe methylene chloride layer was dried over MgSO4
  5. concentrationconcentrated
  6. customthe residue crystallized from isopropyl alcohol and ether
  7. customto give 12.73 g