Dichloromethane → HCID 20085079, compound

HRID 555223Notes

Reaction equation

HRID 555223 reaction equation
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[CH2:3].[Al+3].[Cl-].[Cl-].[Cl-].Cl[CH2:15]Cl>>[CH2:15]1[C:5]2[C:4](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH2:2][CH2:3]1.[CH3:3][C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[CH2:1]

Participants

4

Reactant 3

HCID 6344Dichloromethane2×HCID 7407Alpha-Methylstyrene2×HCID 6451240Aluminum(III) Chloride

Product 1

HCID 20085079HCID 20085079, compound

Procedure

Alpha-methylstyrene (AMS) (2.0 L, 15.4 mole) is added slowly with stirring over 2 to 3 hours to a mixture of AlCl3 (0.7 g, 5.2 mmole) and dichloromethane (1.0 L, dried over 3 Å molecular sieves) in 4 L beaker, in a drybox at room temperature. After the addition of 1 L AMS, about 0.2 L dichloromethane is added to make up for the solvent evaporated due to the reaction exotherm. After the addition of all AMS, the reaction mixture is deactivated with 0.3 L methanol, washed three times with water, dried over calcium chloride, filtered and volatiles stripped first using a rotary evaporator and then high vacuum.

Workup

  1. additionis added
  2. customevaporated due to the reaction exotherm
  3. additionAfter the addition of all AMS
  4. washwashed three times with water
  5. dry with materialdried over calcium chloride
  6. filtrationfiltered
  7. customa rotary evaporator

Sources & evidence

ORD record
ord-7410c399022241e7ad9535a824278918
Source dataset
uspto-grants-2011_11
Patent number
US08053258B2

Reaction notes

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