间苯二酚 → 4-氯甲基-7-羟基苯并吡喃-2-酮

HRID 15645

反应方程式

HRID 15645 反应方程式
[Cl:1][CH2:2][C:3](=O)[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[C:11]1([CH:18]=CC=[C:14](O)[CH:13]=1)[OH:12]>S(=O)(=O)(O)O>[Cl:1][CH2:2][C:3]1[C:9]2[C:8](=[CH:18][C:11]([OH:12])=[CH:13][CH:14]=2)[O:7][C:5](=[O:6])[CH:4]=1

参与物

4

反应物 2

HCID 5054间苯二酚HCID 694844-氯乙酰乙酸乙酯

产物 1

HCID 53988464-氯甲基-7-羟基苯并吡喃-2-酮收率 84%

试剂、催化剂与溶剂 1

HCID 1118四氧化硫溶剂

实验过程

Under ice-cooling, ethyl 4-chloroacetoacetate (14.0 g, 85.0 mmol) was dissolved in concentrated sulfuric acid (30 mL), resorcinol (8.81 g, 80.0 mmol) was added by small portions, and the mixture was stirred at room temperature for 2 hr. The reaction mixture was poured into ice water, and the precipitated solid was collected by filtration, washed with water, and air-dried to give the title compound (14.1 g, yield 84%) as a beige powder.

后处理

  1. temperatureUnder ice-cooling
  2. filtrationthe precipitated solid was collected by filtration
  3. washwashed with water
  4. customair-dried

来源与证据

ORD记录
ord-fe0b5de1698444ec8b5a4db7374edae3
来源数据集
uspto-grants-2010_06
专利号
US07732626B2

关联笔记

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