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

HRID 858272

반응식

HRID 858272 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-592b54ede64b4dbb8ac5bfcd345c18b3
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07148245B2

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