Stannous chloride dihydrate → HCID 70240668, compound

HRID 582768Notes

Reaction equation

HRID 582768 reaction equation
[N:1]([O-])=O.[Na+].Cl.[NH2:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][C:8]=1[CH:16]1[CH2:18][CH2:17]1.O.O.[Cl:21][Sn]Cl>O.Cl.CC(O)=O>[ClH:21].[CH:16]1([C:8]2[CH:9]=[C:10]([CH:14]=[CH:15][C:7]=2[NH:6][NH2:1])[C:11]([OH:13])=[O:12])[CH2:17][CH2:18]1

Participants

7

Reactant 3

HCID 61436Stannous chloride dihydrateHCID 23668193Sodium NitriteHCID 70245388HCID 70245388, compound

Product 1

HCID 70240668HCID 70240668, compoundYield 98.4%

Reagents, catalysts & solvents 3

HCID 176Acetic AcidSolventHCID 313Hydrochloric AcidSolvent2×HCID 962WaterSolvent

Conditions

Temperature
0 °C

Procedure

A solution of 0.38 g of NaNO2 in 4.5 ml of water is added slowly to a solution, cooled to -5° C., of 0.95 g of the product obtained in step C in 22 ml of concentrated HCl and 21 ml of AcOH, and the mixture is stirred for 1 h 15 min at 0° C. It is cooled to -10° C., and a solution of 3.76 g of SnCl2.2H2O in 8 ml of concentrated HCl is added slowly. After 4 hours of stirring at RT, the mixture is filtered, and the residue is washed with 2 ml of concentrated HCl and dried under vacuum to obtain 1 g of expected product.

Workup

  1. temperatureIt is cooled to -10° C.
  2. stirringAfter 4 hours of stirring at RT
  3. filtrationthe mixture is filtered
  4. washthe residue is washed with 2 ml of concentrated HCl
  5. customdried under vacuum

Sources & evidence

ORD record
ord-e51105ae1a6b490e885065164e6b97d1
Source dataset
uspto-grants-1999_07
Patent number
US05925661

Reaction notes

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