1-Methylpiperazine → HCID 22674219, compound

HRID 1005663Notes

Reaction equation

HRID 1005663 reaction equation
[C:1]1([S:7]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13](Cl)[C:12]=2[N+:18]([O-:20])=[O:19])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:21][N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1>>[C:1]1([S:7]([CH2:10][C:11]2[C:12]([N+:18]([O-:20])=[O:19])=[C:13]([N:25]3[CH2:26][CH2:27][N:22]([CH3:21])[CH2:23][CH2:24]3)[CH:14]=[CH:15][CH:16]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

3

Reactant 2

HCID 531671-MethylpiperazineHCID 132569471-[(Benzenesulfonyl)methyl]-3-chloro-2-nitrobenzene

Product 1

HCID 22674219HCID 22674219, compound

Conditions

Temperature
80 °C

Procedure

10 g of 1-benzenesulfonylmethyl-3-chloro-2-nitro-benzene were slurried in 25 mL N-methylpiperazine under nitrogen and stirred. The mixture was heated to 80° C. (oil bath temperature) for a period of 14 hours. The reaction was quenched at 80° C. with 125 mL water, and the thick slurry was filtered, washed with 100 mL water and 100 mL hexanes., and vacuum dried at 45° C. under nitrogen purge for 4 hours, to yield 11.7 g of 1-(3-benzenesulfonylmethyl-2-nitro-phenyl)-4-methyl-piperazine mp 180-182° C.

Workup

  1. customThe reaction was quenched at 80° C. with 125 mL water
  2. filtrationthe thick slurry was filtered
  3. washwashed with 100 mL water and 100 mL hexanes
  4. custom, and vacuum dried at 45° C. under nitrogen
  5. custompurge for 4 hours

Sources & evidence

ORD record
ord-d7e559f4229841cea0b931e643f73767
Source dataset
uspto-grants-2004_09
Patent number
US06787535B2

Reaction notes

Loading…