1,2-Dichloroethane → 6-Bromo-1,1,4,4,7-pentamethyl-1,2,3,4-tetrahydronaphthalene

HRID 858272ノート

反応式

HRID 858272 の反応式
Cl[C:2]([CH3:10])([CH2:4][CH2:5][C:6](Cl)([CH3:8])[CH3:7])[CH3:3].[Br:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH3:18].ClCCCl.[Cl-].[Al+3].[Cl-].[Cl-]>O>[Br:11][C:12]1[CH:17]=[C:16]2[C:15](=[CH:14][C:13]=1[CH3:18])[C:6]([CH3:8])([CH3:7])[CH2:5][CH2:4][C:2]2([CH3:10])[CH3:3]

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 72362-BromotolueneHCID 80360Hexane, 2,5-dichloro-2,5-dimethyl-HCID 6451240Aluminum(III) Chloride

生成物 1

HCID 100393466-Bromo-1,1,4,4,7-pentamethyl-1,2,3,4-tetrahydronaphthalene

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

18.31 g (100.0 mmol) of 2,5-dichloro-2,5-dimethylhexane, 17.10 g (100.0 mmol) of 2-bromotoluene and 200 ml of 1,2-dichloroethane are introduced into a three-necked flask under an argon atmosphere. 1.33 g (10.0 mmol) of aluminium chloride are added rapidly in a single portion and the reaction medium is stirred for thirty minutes at room temperature. The reaction medium is poured into water, extracted with dichloromethane and washed with water, and the organic phase is separated out after settling has taken place, dried over magnesium sulphate and evaporated. After recrystallization of the residue from methanol, 17.78 g (63%) of the expected compound are collected in the form of fine white crystals with a melting point of 73° C.

後処理

  1. extractionextracted with dichloromethane
  2. washwashed with water
  3. customthe organic phase is separated out after settling
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. customAfter recrystallization of the residue from methanol, 17.78 g (63%) of the expected compound
  7. customare collected in the form of fine white crystals with a melting point of 73° C.

出典と根拠

ORDレコード
ord-592b54ede64b4dbb8ac5bfcd345c18b3
出典データセット
uspto-grants-2006_12
特許番号
US07148245B2

反応ノート

読み込み中…