تفاعل #2199946

معادلة التفاعل

Lithium aluminum hydride

tert-butyl 4-morpholin-2-ylmethylpiperazinecarboxylate

sodium hydroxide

chloroform

→

title compound

المردود 66.0%

2-(4-methylpiperazin-1-ylmethyl)morpholine

المردود 66.0%

المذيبات

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   أخرىprepared as an intermediate
2. 2
   workup.ADDITIONadded dropwise under ice-
3. 3
   درجة الحرارةcooling
4. 4
   درجة الحرارةunder reflux for two hours
5. 5
   درجة الحرارةcooling
6. 6
   أخرىfollowed by separation
7. 7
   تجفيفThe organic layer was dried over anhydrous magnesium sulfate
8. 8
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

الإجراء التجريبي

Lithium aluminum hydride (150 mg, 4.10 mmol) was suspended in tetrahydrofuran (5 mL), and the suspension was mixed with a solution of tert-butyl 4-morpholin-2-ylmethylpiperazinecarboxylate (390 mg, 1.37 mmol) prepared as an intermediate according to Process Step 2 of Reference Example 19 in tetrahydrofuran (5 mL) added dropwise under ice-cooling, followed by heating at 60° C. under reflux for two hours. An aqueous sodium hydroxide solution (2 mol/L, 10 mL) and chloroform (50 mL) were added under ice-cooling, followed by separation. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure, to thereby yield the title compound (180 mg, in a yield of 66%).

المصدر