Bromine → HCID 67400551, compound

HRID 912894Notes

Reaction equation

HRID 912894 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-edb0523948154741ae1de81523e8ea3a
Source dataset
uspto-grants-2011_09
Patent number
US08026241B2

Reaction notes

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