Trichloroacetyl chloride → HCID 13067102, compound

HRID 2296308Notes

Reaction equation

HRID 2296308 reaction equation
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[C:6]3[C:7](=[CH:18][NH:19][C:20]=3[CH3:21])[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:24][C:25]([Cl:30])([Cl:29])[C:26](Cl)=[O:27]>C(Cl)Cl>[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[C:6]3[C:7](=[C:18]([C:26]([C:25]([Cl:30])([Cl:29])[Cl:24])=[O:27])[NH:19][C:20]=3[CH3:21])[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 13067095HCID 13067095, compound

Product 1

HCID 13067102HCID 13067102, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture of 3.4 g (11 mmole) of 8-chloro-6-(2-fluorophenyl)-1-methyl-2H,4H-pyrrolo[3,4-d][2]benzazepine, 2.6 g (14 mmole) of trichloroacetyl chloride, and 100 ml of methylene chloride was stirred at room temperature for 12 hr. The resulting precipitate was collected by filtration, resuspended in methylene chloride, and basified with ammonium hydroxide. The methylene chloride solution was separated, dried over anhydrous sodium sulfate, and concentrated at reduced pressure to give a (mp 222°-225°) colorless solid. A small portion was recrystallized from a mixture of methylene chloride and ether to give colorless prisms, mp 222°-223°.

Workup

  1. filtrationThe resulting precipitate was collected by filtration
  2. customThe methylene chloride solution was separated
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated at reduced pressure

Sources & evidence

ORD record
ord-de8ff126315d46ba8b0eab791aab80f2
Source dataset
uspto-grants-1984_01
Patent number
US04428879

Reaction notes

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