Stannous chloride dihydrate → HCID 18184747, compound

HRID 1358379Notes

Reaction equation

HRID 1358379 reaction equation
[CH3:1][C:2]1([CH3:18])[CH2:7][C:6]([CH3:9])([CH3:8])[CH2:5][CH:4]([O:10][C:11]2[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=2)[CH2:3]1.[N:19]([O-])=O.[Na+].O.O.[Sn](Cl)[Cl:26]>O.Cl>[ClH:26].[CH3:9][C:6]1([CH3:8])[CH2:7][C:2]([CH3:18])([CH3:1])[CH2:3][CH:4]([O:10][C:11]2[CH:12]=[CH:13][C:14]([NH:15][NH2:19])=[CH:16][CH:17]=2)[CH2:5]1

Participants

6

Reactant 3

HCID 61436Stannous chloride dihydrateHCID 18184759HCID 18184759, compoundHCID 23668193Sodium Nitrite

Product 1

HCID 18184747HCID 18184747, compound

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolvent2×HCID 962WaterSolvent2×

Conditions

Temperature
-10 °C

Procedure

A stirred mixture, cooled to −10° C., of 3.7 g of 4-(3,3,5,5-tetramethylcyclohexyloxy)aniline, 7.5 ml of water and 15.5 ml of conc. HCl is mixed dropwise with a solution of 1.13 g of sodium nitrite in 7.5 ml of water, and the mixture is stirred at −10° C. for 45 min and subsequently added dropwise to a suspension of 9.3 g of tin dichloride dihydrate in 7 ml of conc. HCl. The precipitate is filtered off with suction, washed with water, suspended under nitrogen in 200 ml of water and decomposed at 10-15° C. using 100 ml of 30% strength aqueous sodium hydroxide solution. The precipitate that is then formed is filtered off with suction, washed with water, taken up in 200 ml of ether and dried with sodium sulfate. The product is precipitated using ethereal HCl, filtered off with suction and dried under reduced pressure.

Workup

  1. filtrationThe precipitate is filtered off with suction
  2. washwashed with water
  3. customdecomposed at 10-15° C.
  4. customThe precipitate that is then formed
  5. filtrationis filtered off with suction
  6. washwashed with water
  7. dry with materialdried with sodium sulfate
  8. customThe product is precipitated
  9. filtrationfiltered off with suction
  10. customdried under reduced pressure

Sources & evidence

ORD record
ord-dc79c998870f4210b6c8c94911beef4a
Source dataset
uspto-grants-2003_07
Patent number
US06596742B1

Reaction notes

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