Acetic Anhydride → HCID 20402703, compound

HRID 1980268Notes

Reaction equation

HRID 1980268 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

  1. concentrationwas concentrated to dryness under vacuum
  2. additiontreated with charcoal
  3. concentrationBy concentrating to a volume of 600 ml
  4. temperaturecooling
  5. 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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