تفاعل #354952

معادلة التفاعل

lithium aluminum hydride

3-hydroxy-3-formamidomethyl-3,4-dihydro-2H-1,5-benzodioxepin

hydrochloric acid

lithium aluminum hydride

sodium hydroxide

3-hydroxy-3-methylaminomethyl-3,4-dihydro-2H-1,5-benzodioxepin hydrochloride

→

3-methylaminomethyl-3,4-dihydro-2H-1,5-benzodioxepin hydrochloride

المذيبات

ether

ether

ethanol

water

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture then is refluxed for 2 hours
2. 2
   أخرىThe white solid formed
3. 3
   ترشيحis filtered
4. 4
   تجفيفthe filtrate dried over magnesium sulfate
5. 5
   أخرىIt is stripped affording 3.8 g
6. 6
   أخرىto give 3.7 g
7. 7
   أخرىrecrystallizations from ethanol

الإجراء التجريبي

3-hydroxy-3-formamidomethyl-3,4-dihydro-2H-1,5-benzodioxepin (5.8 g.) in 200 ml. anhydrous ether is added to lithium aluminum hydride (2.0 g.) in 40 ml. of anhydrous ether dropwise in one hour. The mixture then is refluxed for 2 hours and the excess lithium aluminum hydride then decomposed with water (5.0 ml.) followed by 10% sodium hydroxide (3.6 ml.) followed by 6.0 ml. of water. The white solid formed is filtered and the filtrate dried over magnesium sulfate then over calcium sulfate. It is stripped affording 3.8 g. of oil. The oil is acidified with 11N hydrochloric acid in ethanol to give 3.7 g. of 3-hydroxy-3-methylaminomethyl-3,4-dihydro-2H-1,5-benzodioxepin hydrochloride, m.p. 189°-205°C. Following several recrystallizations from ethanol, the product melts at 217-219°C.

المصدر