HRID2415463

反应详情

EQUATION

反应方程式

HRID 2415463 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
250 °C

PROCEDURE

实验过程

3.67 g (11.8 mmol) of 3-(3-benzyloxy-phenylamino)-but-2-enoic acid ethyl ester were added dropwise within 20 minutes to 5.5 ml of Dowtherm A heated at 250° C. (metal bath temperature). The solution was stirred further 10 minutes at 250° C. (bath temperature), cooled to RT and then treated with 20 ml of heptane. The brown viscous oil that had formed was isolated and triturated with 45 ml of AcOEt. The brown solid obtained was filtered off by suction, washed with AcOEt and dried in a high vacuum to give 1.19 g (35%) of 7-benzyloxy-2-methyl-quinolin-4-ol. ISP mass spectrum, m/e: 266.3 (M+1 calculated for C17H15NO2: 266).

WORKUP

后处理

  1. temperaturecooled to RT
  2. customThe brown viscous oil that had formed
  3. customwas isolated
  4. customtriturated with 45 ml of AcOEt
  5. customThe brown solid obtained
  6. filtrationwas filtered off by suction
  7. washwashed with AcOEt
  8. customdried in a high vacuum