HRID1052335

反应详情

EQUATION

反应方程式

HRID 1052335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

was prepared as described in Example II of U.S. Pat. No. 6,590,082, which is hereby incorporated by reference herein in its entirety. A mixture of octadecanol (270 grams, 1.0 mol; obtained from Sigma-Aldrich Co., Milwaukee, Wis.), isatoic anhydride (24 grams, 1.5 mol; obtained from Sigma-Aldrich Co.), and 1,4-diazabicyclo[2.2.2]octane (56 grams, 0.50 mol; obtained from Sigma-Aldrich Co.) in 1,000 milliliters of dimethylformamide was stirred and heated to 100° C. in a 4 liter beaker. Vigorous gas evolution occurred. After 10 minutes, the resultant brown solution was heated to 150° C. for 15 minutes. The reaction mixture was then cooled to 50° C. and vigorously stirred while 3,000 milliliters of methanol was added. The resultant suspension was stirred for 0.5 hour followed by vacuum filtration. The solid thus obtained was washed in the filter funnel with 4×300 milliliter portions of methanol and then dried in air to give the product stearyl anthranilate as white power (330.5 grams, 85 percent yield).

WORKUP

后处理

  1. customwas prepared
  2. temperaturethe resultant brown solution was heated to 150° C. for 15 minutes
  3. temperatureThe reaction mixture was then cooled to 50° C.
  4. additionwas added
  5. filtrationfollowed by vacuum filtration
  6. customThe solid thus obtained
  7. washwas washed in the filter funnel with 4×300 milliliter portions of methanol
  8. customdried in air