Stannous chloride dihydrate → HCID 10631005, compound

HRID 1781053Notes

Reaction equation

HRID 1781053 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([C:6]([N+:11]([O-])=O)=[CH:7][C:8]=1[CH2:9][CH3:10])[NH2:5].O.O.Cl[Sn]Cl>>[NH2:11][C:6]1[CH:7]=[C:8]([CH2:9][CH3:10])[C:2]([Cl:1])=[CH:3][C:4]=1[NH2:5]

Participants

3

Reactant 2

HCID 61436Stannous chloride dihydrateHCID 21189944HCID 21189944, compound

Product 1

HCID 10631005HCID 10631005, compoundYield 99.4%

Procedure

A solution of 271 mg (1.35 mmol) of 34 and 1.24 g (5.49 mmol) of SnCl2.2H2O, in 5 mL of absolute alcohol was refluxed for 2 h. It was evaporated and the residue was treated with 1N NaOH to pH=10. The mixture was extracted with CH2Cl2 (3×10 mL). The extract was dried (MgSO4) and evaporated to leave 229 mg (99%) of a yellow solid. 1H NMR (CDCl3), 1.165 (t, 3, J=7.5), 2.594 (q, 2, J=7.2), 6.560 (s, 1), 6.696 (s, 1).

Workup

  1. customIt was evaporated
  2. additionthe residue was treated with 1N NaOH to pH=10
  3. extractionThe mixture was extracted with CH2Cl2 (3×10 mL)
  4. dry with materialThe extract was dried (MgSO4)
  5. customevaporated

Sources & evidence

ORD record
ord-7be7b329106841c5a1cdf0b795ef6837
Source dataset
uspto-grants-1997_05
Patent number
US05631373

Reaction notes

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