Acetic Anhydride → HCID 20402703, compound
Reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9]2[C:10](=[CH:18][N:19]([CH3:22])[C:20]=2[CH3:21])[N:11]([CH3:17])[C:12](=[O:16])[CH2:13][N+:14]=1[O-].[C:23]([O:26]C(=O)C)(=[O:25])[CH3:24]>>[C:23]([O:26][CH:13]1[C:12](=[O:16])[N:11]([CH3:17])[C:10]2=[CH:18][N:19]([CH3:22])[C:20]([CH3:21])=[C:9]2[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Cl:1])=[N:14]1)(=[O:25])[CH3:24]Participants
3
Conditions
- Temperature
- 55 °C
Procedure
The compound obtained in step (d) above was suspended in acetic anhydride (660 ml) and the reaction flask was heated in a water-bath at 55° C. After stirring for 15 minutes the reaction mixture was concentrated to dryness under vacuum, and the obtained residue was taken up with boiling ethanol and treated with charcoal. By concentrating to a volume of 600 ml and cooling, the compound of the title (103 g) crystallized. M.p. 202°-4° C.
Workup
- concentrationwas concentrated to dryness under vacuum
- additiontreated with charcoal
- concentrationBy concentrating to a volume of 600 ml
- temperaturecooling
- customthe compound of the title (103 g) crystallized
Sources & evidence
- ORD record
- ord-935310cb1be14c808b5cc26a643daa2c
- Source dataset
- uspto-grants-1985_04
- Patent number
- US04508730
Reaction notes
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