Water → HCID 67042000, compound

HRID 1929289Notes

Reaction equation

HRID 1929289 reaction equation
[Br:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[C:4]([N+:12]([O-:14])=[O:13])[C:3]=1[NH:15][CH2:16][C:17]([CH3:20])([CH3:19])[CH3:18].O.[OH-].[Li+]>O1CCCC1>[Br:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[C:4]([N+:12]([O-:14])=[O:13])[C:3]=1[NH:15][CH2:16][C:17]([CH3:20])([CH3:19])[CH3:18]

Participants

5

Reactant 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 67041941HCID 67041941, compound

Product 1

HCID 67042000HCID 67042000, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

0.88 g (2.55 mmol) of methyl 4-bromo-3-[(2,2-dimethylpropyl)amino]-2-nitrobenzoate was dissolved in 10 ml of tetrahydrofuran and 10 ml of water and admixed with 0.064 g (2.67 mmol) of lithium hydroxide. The mixture was left with stirring for 15 h and then concentrated. The residue was taken up in water and washed with methylene chloride and the aqueous phase was adjusted to a pH of 1 using a KHSO4 solution. The precipitate was isolated by filtration with suction, washed with water and dried under reduced pressure at 70° C.

Workup

  1. waitThe mixture was left
  2. concentrationconcentrated
  3. washwashed with methylene chloride
  4. customThe precipitate was isolated by filtration with suction
  5. washwashed with water
  6. customdried under reduced pressure at 70° C.

Sources & evidence

ORD record
ord-34359177ad614ecbab6906d3f3e144bd
Source dataset
uspto-grants-2012_05
Patent number
US08188002B2

Reaction notes

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