Toluene → Toluene dimethoxyethane
Reaction equation
[C:1]1([CH3:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:8][O:9][CH2:10][CH2:11][O:12][CH3:13]>>[CH3:8][O:9][CH2:10][CH2:11][O:12][CH3:13].[C:1]1([CH3:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1Participants
3
Procedure
A saturated solution of compound of formula (I), Form VI in 1,2-dimethoxyethane was made at room temperature by adding 1.4 mL of 1,2-dimethoxyethane to approximately 698 mg of Form VI. The saturated solution was stirred for approximately 1 h and subsequently filtered through a filter of 0.45 μm pore size. A reverse addition of 200 μL of the as prepared saturated solution was added at once to 800 μL of toluene acting as anti-solvent. After precipitation the solid material was separated from solution and analyzed as described in Table 1. No drying under vacuum was applied prior to the analyses.
Workup
- customwas made at room temperature
- filtrationsubsequently filtered through
- filtrationa filter of 0.45 μm pore size
- additionA reverse addition of 200 μL of the
- customas prepared saturated solution
- customAfter precipitation the solid material
- customwas separated from solution
Sources & evidence
- ORD record
- ord-0ee8d7016dc64ec9aad86f2e6a651708
- Source dataset
- uspto-grants-2013_09
- Patent number
- US08541391B2
Reaction notes
Loading…