Bromine → HCID 67400551, compound

HRID 730835Notes

Reaction equation

HRID 730835 reaction equation
[F:1][C:2]([F:16])([F:15])[C:3]1[C:4]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[N:5][CH:6]=[CH:7][CH:8]=1.[Br:17]Br>ClCCl>[Br:17][C:7]1[CH:8]=[C:3]([C:2]([F:1])([F:15])[F:16])[C:4]([N:9]2[CH2:10][CH2:11][NH:12][CH2:13][CH2:14]2)=[N:5][CH:6]=1

Participants

4

Reactant 2

HCID 24408BromineHCID 27777861-[3-(Trifluoromethyl)pyridin-2-yl]piperazine

Product 1

HCID 67400551HCID 67400551, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of 1-(3-trifluoromethyl-pyridin-2-yl)-piperazine (8 g, 34.6 mmol, Oakwood) in dichloromethane (230 mL) was added dropwise bromine (3.92 mL, 76.12 mmol, Aldrich) with stirring at room temperature. The resulting mixture was stirred at room temperature for 16 h and the precipitate was filtered, washed with EtOAc (2×100 mL) and dried in vacuo to give the title compound as a yellow solid, which was used in the next step without additional purification. MS (ESI, positive ion) m/z: 310 (M+1).

Workup

  1. stirringThe resulting mixture was stirred at room temperature for 16 h
  2. filtrationthe precipitate was filtered
  3. washwashed with EtOAc (2×100 mL)
  4. customdried in vacuo

Sources & evidence

ORD record
ord-bf332eb6b149435a87a775c9af97f59d
Source dataset
uspto-grants-2009_09
Patent number
US07582761B2

Reaction notes

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