Acetic Anhydride → HCID 13556939, compound

HRID 464184Notes

Reaction equation

HRID 464184 reaction equation
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[C:6]3[N:22]=[CH:21][N:20]=[CH:19][C:7]=3[CH2:8][N+:9]([O-])=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[F:17])[C:4]=2[CH:3]=1.[C:25]([O:28]C(=O)C)(=[O:27])[CH3:26]>>[C:25]([O:28][CH:8]1[C:7]2[CH:19]=[N:20][CH:21]=[N:22][C:6]=2[C:5]2[CH:23]=[CH:24][C:2]([Cl:1])=[CH:3][C:4]=2[C:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[F:17])=[N:9]1)(=[O:27])[CH3:26]

Participants

3

Reactant 2

HCID 7918Acetic AnhydrideHCID 13225510HCID 13225510, compound

Product 1

HCID 13556939HCID 13556939, compound

Procedure

A mixture of 2.5 g (7.4 mmoles) of 9-chloro-7-(2-fluorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-6-oxide and 50 ml of acetic anhydride was heated on the steambath for 24 hours. The reaction mixture was concentrated at reduced pressure to dryness and the residue was crystallized from a mixture of methylene chloride and ether to give the crude product, m.p. 197°-198° C. Recrystallization from a mixture of methylene chloride and ether gave the pure product as cream colored prisms, m.p. 200°-201° C.

Workup

  1. temperaturewas heated on the steambath for 24 hours
  2. concentrationThe reaction mixture was concentrated at reduced pressure to dryness
  3. customthe residue was crystallized from a mixture of methylene chloride and ether

Sources & evidence

ORD record
ord-245dc990a6b04560a27d2b69fe47f4df
Source dataset
uspto-grants-1985_10
Patent number
US04546183

Reaction notes

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