反应 #157353

反应方程式

HCl

1,4-dioxane

tert-butyl 4-(5-(2-chlorophenyl)furan-2-carbonyl)-3-((pyridin-3-yloxy)methyl)piperazine-1-carboxylate TFA salt

→

desired product

收率 59.0%

(5-(2-chlorophenyl)furan-2-yl)(2-((pyridin-3-yloxy)methyl)piperazin-1-yl)methanone dihydrochloride

收率 59.0%

溶剂

MeOH

反应条件

后处理

1. 1
   浓缩the reaction mixture was concentrated under reduced pressure
2. 2
   其他purified by HPLC (5 to 50% MeCN/0.1% TFA in H2O/0.1% TFA gradient)
3. 3
   浓缩The desired chromatography fractions were concentrated under reduced pressure
4. 4
   workup.DISSOLUTIONdissolved in MeOH (1 mL)
5. 5
   workup.ADDITIONtreated with 4 M HCl in 1,4-dioxane (6 mL)
6. 6
   浓缩This was concentrated under reduced pressure

实验过程

4 M HCl in 1,4-dioxane (6 mL, 24 mmol) was added to a solution of tert-butyl 4-(5-(2-chlorophenyl)furan-2-carbonyl)-3-((pyridin-3-yloxy)methyl)piperazine-1-carboxylate TFA salt (66.6 mg, 0.109 mmol) in MeOH (1 mL). After 1 h, the reaction mixture was concentrated under reduced pressure and purified by HPLC (5 to 50% MeCN/0.1% TFA in H2O/0.1% TFA gradient). The desired chromatography fractions were concentrated under reduced pressure, dissolved in MeOH (1 mL), and treated with 4 M HCl in 1,4-dioxane (6 mL). This was concentrated under reduced pressure, yielding 30 mg (59%) of the desired product as a white solid. LC-MS: RT=5.00 min, [M+H]+=398.1.

来源