反应详情

NaOCH3 30% (0.592 mole) was added to a solution of hydroxylamine hydrochloride (0.1085 mole) in CH3OH (200 ml), stirred at RT. The mixture was stirred for 10 minutes. Intermediate (3) (0.0542 mole) was added portionwise and the resulting reaction mixture was stirred and refluxed overnight. The solvent was evaporated. The residue was partitioned between CH2Cl2 and water. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was stirred in DIPE, filtered off, washed with DIPE, and dried, yielding 3.7 g (26%) of 4-amino-2,6-dichloro-N′-hydroxy-α,α-dimethylbenzeneethanimidamide (intermediate 17).

1. stirringThe mixture was stirred for 10 minutes
2. customthe resulting reaction mixture
3. stirringwas stirred
4. temperaturerefluxed overnight
5. customThe solvent was evaporated
6. customThe residue was partitioned between CH2Cl2 and water
7. customThe organic layer was separated
8. customdried
9. filtrationfiltered
10. customthe solvent was evaporated
11. stirringThe residue was stirred in DIPE
12. filtrationfiltered off
13. washwashed with DIPE
14. customdried