Stannous chloride dihydrate → HCID 22111820, compound

HRID 582763Notes

Reaction equation

HRID 582763 reaction equation
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][C:3]=1[CH3:11].[N:12]([O-])=O.[Na+].O.O.[Cl:18][Sn]Cl>Cl.O>[ClH:18].[NH:1]([C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][C:3]=1[CH3:11])[NH2:12]

Participants

6

Reactant 3

HCID 61436Stannous chloride dihydrateHCID 121180574-amino-3-methylbenzamideHCID 23668193Sodium Nitrite

Product 1

HCID 22111820HCID 22111820, compoundYield 58.1%

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolvent3×HCID 962WaterSolvent

Conditions

Temperature
0 °C

Procedure

0.5 g of the compound of step A is dissolved in 10 ml of 1N HCl and 5 ml of concentrated HCl. The mixture is cooled to 0° C. and a solution of 230 mg of NaNO2 in 3 ml of water is added. After 15 minutes at -10° C., a solution of 1.5 g of SnCl2.2H2O in 5 ml of concentrated HCl is added. After 1 hour the precipitate is filtered off and dried under vacuum over P2O5 to obtain 390 mg of the expected product.

Workup

  1. filtrationAfter 1 hour the precipitate is filtered off
  2. dry with materialdried under vacuum over P2O5

Sources & evidence

ORD record
ord-0175efe60e7c467b80d99273b1d99146
Source dataset
uspto-grants-1999_07
Patent number
US05925661

Reaction notes

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