تفاعل #51271

معادلة التفاعل

2,5-dichloro-2,5-dimethylhexane

dichloromethane

ammonium chloride

dichloromethane

3-bromophenol

→

3-bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphth1-ol

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONis added dropwise
2. 2
   استخلاصextracted with dichloromethane
3. 3
   غسيلthe extract is washed with water
4. 4
   أخرىthe organic phase is separated
5. 5
   تجفيفdried over magnesium sulphate
6. 6
   أخرىevaporated
7. 7
   أخرىThe residue obtained
8. 8
   أخرىis purified by chromatography on a silica column
9. 9
   غسيلeluted with a mixture
10. 10
    أخرىAfter evaporating the solvents, 30.00 g (53%) of the expected compound
11. 11
    أخرىare collected in the form of white crystals with a melting point of 93° C.

الإجراء التجريبي

13.40 g (100.0 mmol) of ammonium chloride and 100 ml of dichloromethane are introduced into a three-necked flask under an argon atmosphere. A solution composed of 34.60 g (199.0 mmol) of 3-bromophenol, 89.00 g (486.0 mmol) of 2,5-dichloro-2,5-dimethylhexane and 300 ml of dichloromethane is added dropwise. The reaction mixture is stirred for sixteen hours at room temperature. The reaction mixture is poured into water and extracted with dichloromethane, the extract is washed with water and the organic phase is separated by settling, dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a silica column eluted with a mixture composed of 80% heptane and 20% dichloromethane. After evaporating the solvents, 30.00 g (53%) of the expected compound are collected in the form of white crystals with a melting point of 93° C.

المصدر