Stannous chloride dihydrate → HCID 70127080, compound

HRID 651379Notes

Reaction equation

HRID 651379 reaction equation
[CH2:1]([O:8][C:9](=[O:22])[NH:10][C:11]1[C:16]([N+:17]([O-])=O)=[CH:15][CH:14]=[CH:13][C:12]=1[O:20][CH3:21])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.O.Cl[Sn]Cl>C(O)C>[CH2:1]([O:8][C:9](=[O:22])[NH:10][C:11]1[C:12]([O:20][CH3:21])=[CH:13][CH:14]=[CH:15][C:16]=1[NH2:17])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 61436Stannous chloride dihydrateHCID 70127773HCID 70127773, compound

Product 1

HCID 70127080HCID 70127080, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
70 °C

Procedure

A mixture of (2-methoxy-6-nitrophenyl) carbamic acid benzyl ester (17.5 g; 0.058 mol) and SnCl2·2H2O (65.3 g; 0.29 mol) in anhydrous ethanol, was heated at 70° C. for 2 hours. The solvent was then removed under vacuum and the residue was acidified with 10% aqueous HCl. The title compound was extracted with ethyl acetate and washed with diluted aqueous K2CO3. The precipitated solid was filtered off, the organic layer was dried over MgSO4 and evaporated under vacuum to give the title compound after crystallization with n-hexane. The compound was used without further purification. Yellow solid; 9.6 g.

Workup

  1. customThe solvent was then removed under vacuum
  2. extractionThe title compound was extracted with ethyl acetate
  3. washwashed with diluted aqueous K2CO3
  4. filtrationThe precipitated solid was filtered off
  5. dry with materialthe organic layer was dried over MgSO4
  6. customevaporated under vacuum

Sources & evidence

ORD record
ord-34323475c0304afa9e3dc85dc7ab6a41
Source dataset
uspto-grants-2001_08
Patent number
US06281218B1

Reaction notes

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