三氯氧磷 → 1-氯异喹啉

HRID 1181406

反应方程式

HRID 1181406 反应方程式
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][N+:2]=1[O-].P(Cl)(Cl)([Cl:14])=O>ClCCl>[Cl:14][C:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][N:2]=1

参与物

4

反应物 2

HCID 24813三氯氧磷HCID 290378异喹啉-N-氧化物

产物 1

HCID 1405391-氯异喹啉

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂2 次

实验过程

A solution of isoquinoline-N-oxide (5.52 g, 38 mmol) in dichloromethane (50 ml) was added over 15 minutes to a solution of phosphorus oxychloride (40 ml) in dichloromethane (50 ml) at room temperature. The mixture was stirred for 1 hour, then heated to reflux for 2 hours. After cooling to room temperature, the mixture was poured into ice water (500 ml). The mixture was then extracted with dichloromethane (2×250 ml) and the combined organic layers were washed with 10% aqueous potassium carbonate solution (200 ml), brine (200 ml) then dried (Na2SO4) and evaporated to give the title compound (5.0 g).

后处理

  1. temperatureheated
  2. temperatureto reflux for 2 hours
  3. extractionThe mixture was then extracted with dichloromethane (2×250 ml)
  4. washthe combined organic layers were washed with 10% aqueous potassium carbonate solution (200 ml), brine (200 ml)
  5. dry with materialthen dried (Na2SO4)
  6. customevaporated

来源与证据

ORD记录
ord-b036090dc2e549a78f27e7912803a8ce
来源数据集
uspto-grants-2007_10
专利号
US07285563B2

关联笔记

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