Hydroxyamine hydrochloride → HCID 58446972, compound

HRID 1045773Notes

Reaction equation

HRID 1045773 reaction equation
[Br:1][C:2]1[C:3]([N:21]=[CH:22][N:23](C)C)=[N:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1.Cl.N[OH:28]>CO>[Br:1][C:2]1[C:3]([N:21]=[CH:22][NH:23][OH:28])=[N:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1

Participants

4

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 58447035HCID 58447035, compound

Product 1

HCID 58446972HCID 58446972, compoundYield 80%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A 100 mL round bottom flask was charged with tert-butyl 4-(5-bromo-4-(((dimethylamino)methylene)amino)pyrimidin-2-yl)piperazine-1-carboxylate (2.0 g) and methanol (30 mL). To the above solution was added hydroxylamine hydrochloride (0.5 g, 7.3 mmol) in one portion. The resulting mixture was stirred at room temperature for 12 h. Work-up: the solvent was evaporated. The resulting crystalline solid was washed with water and collected by filtration. The solid was washed with ethanol (100 mL) and dried, to afford 1.0 g (80%) of the product as a white solid.

Workup

  1. customthe solvent was evaporated
  2. washThe resulting crystalline solid was washed with water
  3. filtrationcollected by filtration
  4. washThe solid was washed with ethanol (100 mL)
  5. customdried

Sources & evidence

ORD record
ord-f21145a0dee544949b45b2a072cc5e23
Source dataset
uspto-grants-2013_10
Patent number
US08569300B2

Reaction notes

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