Water → HCID 67041952, compound

HRID 1929286Notes

Reaction equation

HRID 1929286 reaction equation
[Cl:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8]CC)=[O:7])=[C:4]([N+:13]([O-:15])=[O:14])[C:3]=1[NH:16][CH3:17].O.[OH-].[Li+]>O1CCCC1>[Cl:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([OH:8])=[O:7])=[C:4]([N+:13]([O-:15])=[O:14])[C:3]=1[NH:16][CH3:17]

Participants

5

Reactant 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 67042273HCID 67042273, compound

Product 1

HCID 67041952HCID 67041952, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

3.01 g (11.6 mmol) of ethyl 4-chloro-3-(methylamino)-2-nitrobenzoate were dissolved in 35 ml of tetrahydrofuran and 22 ml of water and this solution was admixed with 0.5 g (20.9 mmol) of lithium hydroxide. It was left with stirring for 8 h and then concentrated. The residue was taken up in water and washed with methylene chloride, and the aqueous phase was then 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. waitIt 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-09509869bbe64cf2921bf3f9dc16741f
Source dataset
uspto-grants-2012_05
Patent number
US08188002B2

Reaction notes

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