Triphosgene → 5,6-Dimethoxyisatoic anhydride
Reaction equation
[NH2:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[C:6]([O:11][CH3:12])[C:5]([O:13][CH3:14])=[CH:4][CH:3]=1.Cl[C:16](Cl)([O:18]C(=O)OC(Cl)(Cl)Cl)Cl>O1CCCC1>[CH3:12][O:11][C:6]1[C:7]2[C:8](=[O:10])[O:9][C:16](=[O:18])[NH:1][C:2]=2[CH:3]=[CH:4][C:5]=1[O:13][CH3:14]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
10.0 g (50.7 mmol) 6-Amino-2,3-dimethoxy-benzoic acid were dissolved in 150 ml tetrahydrofuran, 6.52 g (22.0 mmol) triphosgene were added and the solution was refluxed for 3 h. After pouring on 400 ml of a ice/water mixture the precipitate was filtrated and rinsed with water and methanol.
Workup
- temperaturethe solution was refluxed for 3 h
- filtrationwas filtrated
- washrinsed with water and methanol
Sources & evidence
- ORD record
- ord-7c2639eeec404c40a486bcc56b86cecf
- Source dataset
- uspto-grants-2011_11
- Patent number
- US08058431B2
Reaction notes
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