Trichloroacetyl chloride → HCID 13067119, compound

HRID 2296319Notes

Reaction equation

HRID 2296319 reaction equation
[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[C:6]3[C:7](=[CH:18][NH:19][CH:20]=3)[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[F:17])[C:4]=2[CH:3]=1.[Cl:23][C:24]([Cl:29])([Cl:28])[C:25](Cl)=[O:26]>C(Cl)Cl>[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[C:6]3[C:7](=[C:18]([C:25](=[O:26])[C:24]([Cl:29])([Cl:28])[Cl:23])[NH:19][CH:20]=3)[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[F:17])[C:4]=2[CH:3]=1

Participants

4

Reactant 2

HCID 6420Trichloroacetyl chlorideHCID 136045442HCID 136045442, compound

Product 1

HCID 13067119HCID 13067119, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture of 0.7 g (2.2 mmol) of 8-chloro-6-(2-fluorophenyl)-2H,4H-pyrrolo[3,4-d][2]benzazepine and 2.0 ml (18 mmol) of trichloroacetyl chloride in 20 ml of methylene chloride was refluxed for 7 days. The resulting precipitate was collected by filtration and partitioned between methylene chloride and saturated aqueous sodium bicarbonate. The methylene chloride solution was dried over anhydrous sodium sulfate and concentrated at reduced pressure to give a white solid mp 240°-245° (dec).

Workup

  1. temperaturewas refluxed for 7 days
  2. filtrationThe resulting precipitate was collected by filtration
  3. custompartitioned between methylene chloride and saturated aqueous sodium bicarbonate
  4. dry with materialThe methylene chloride solution was dried over anhydrous sodium sulfate
  5. concentrationconcentrated at reduced pressure

Sources & evidence

ORD record
ord-a94053e1ddad4efcbbc2a5d496f8dd44
Source dataset
uspto-grants-1984_01
Patent number
US04428879

Reaction notes

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