Trimethyl orthoformate → HCID 68822180, compound
Reaction equation
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH3:11])[C:6]=1[S:7]([NH2:10])(=[O:9])=[O:8].[CH:12](OC)(OC)OC>>[CH3:11][C:5]1[C:6]2[S:7](=[O:8])(=[O:9])[N:10]=[CH:12][NH:1][C:2]=2[S:3][CH:4]=1Participants
3
Conditions
- Temperature
- 90 °C
Procedure
200 mg of 2-amino-4-methylthiophene-3-sulphonamide, the preparation of which is described in patent WO 99/03861, are dissolved in 1.5 ml of trimethyl orthoformate. The mixture is heated at 90° C. for 2 hours in an open vessel. After evaporation of the solvent under reduced pressure, the residue is taken up in 3 ml of ethyl acetate. The resulting insoluble material is collected by filtration, washed with diethyl ether and dried.
Workup
- customAfter evaporation of the solvent under reduced pressure
- filtrationThe resulting insoluble material is collected by filtration
- washwashed with diethyl ether
- customdried
Sources & evidence
- ORD record
- ord-69695625111a4249ada7ca21d0cbfcf6
- Source dataset
- uspto-grants-2009_01
- Patent number
- US07476668B2
Reaction notes
Loading…