Water → HCID 62508285, compound

HRID 2063274Notes

Reaction equation

HRID 2063274 reaction equation
F[C:2]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:3]=1[NH2:4].[CH3:12][CH:13]1[CH2:17][CH2:16][CH2:15][NH:14]1.O>ClCCl>[CH3:12][CH:13]1[CH2:17][CH2:16][CH2:15][N:14]1[C:2]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:3]=1[NH2:4]

Participants

5

Reactant 3

HCID 962WaterHCID 130032-MethylpyrrolidineHCID 677852-Fluoro-5-nitroaniline

Product 1

HCID 62508285HCID 62508285, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
100 °C

Procedure

5 g (32.03 mmol) of 2-fluoro-5-nitroaniline and 4.9 ml (48.04 mmol) of 2-methylpyrrolidine (racemic) are placed in a screw reactor. The reactor is closed and the mixture is heated at 100° C. for 5 h. After cooling, the mixture is taken up with 100 ml of water and 100 ml of dichloromethane. The organic phase is separated, washed with 50 ml of a saturated solution of sodium chloride, dried over magnesium sulphate and then concentrated under reduced pressure. The resulting product is used as it is in the subsequent reaction.

Workup

  1. customThe reactor is closed
  2. temperatureAfter cooling
  3. customThe organic phase is separated
  4. washwashed with 50 ml of a saturated solution of sodium chloride
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated under reduced pressure
  7. customis in the subsequent reaction

Sources & evidence

ORD record
ord-3e93482f0aad41928ddd1994eaeb4b47
Source dataset
uspto-grants-2012_10
Patent number
US08288376B2

Reaction notes

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