反应详情

Thionyl chloride (7.4 ml, 101.5 mmol), dissolved in dichloromethane (50 ml), is added dropwise at 4° C. to a solution of (2-[(3-chloro-2-hydroxymethyl-pyridin-4-yl)-methylamino]-ethanol (10.0 g, 46.1 mmol) in dichloromethane (150 ml). The solution is stirred for 1 h at this temperature, triturated with ice water and neutralized with saturated sodium bicarbonate solution. After separation of the organic layer the aqueous phase is extracted with dichloromethane. The combined organic extracts are washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue is employed without additional purification for the synthesis described in step b).

1. customtriturated with ice water and neutralized with saturated sodium bicarbonate solution
2. customAfter separation of the organic layer the aqueous phase
3. extractionis extracted with dichloromethane
4. washThe combined organic extracts are washed with water
5. dry with materialdried over magnesium sulfate
6. customevaporated in vacuo
7. customThe residue is employed without additional purification for the synthesis