Sodium Carbonate → HCID 178485839, compound

HRID 1696777Notes

Reaction equation

HRID 1696777 reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([NH:8][C:9]([NH:11][CH3:12])=[O:10])[CH:5]=[C:4]([C:13]#[N:14])[CH:3]=1.Cl.[NH2:16][OH:17].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C.O>[NH2:1][C:2]1[CH:3]=[C:4]([CH:5]=[C:6]([NH:8][C:9]([NH:11][CH3:12])=[O:10])[N:7]=1)[C:13]([NH:16][OH:17])=[NH:14]

Participants

6

Reactant 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 67273747HCID 67273747, compound

Product 1

HCID 178485839HCID 178485839, compoundYield 65.7%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Conditions

Temperature
85 °C

Procedure

To a solution of 0.200 g 1-(6-amino-4-cyano-pyridin-2-yl)-3-methyl-urea (example 23a) in 3.2 ml ethanol and 1.6 ml water was added 0.145 g hydroxylamine hydrochloride and 0.333 g sodium carbonate and the mixture was stirred at 85° C. for 2 h. The reaction mixture was purified by solid phase extraction with ethyl acetate to yield 0.154 g of the title compound as light yellow solid. MS (ISP) M+H+=225.1

Workup

  1. customThe reaction mixture was purified by solid phase extraction with ethyl acetate

Sources & evidence

ORD record
ord-e735ad29ad9a4857a5cbbcc8ba9c6083
Source dataset
uspto-grants-2012_04
Patent number
US08163778B2

Reaction notes

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