Sodium Carbonate → HCID 54067653, compound

HRID 1289369Notes

Reaction equation

HRID 1289369 reaction equation
[F:1][C:2]1[C:3]([N+:21]([O-])=O)=[CH:4][C:5]2[N:10]([CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[S:9](=[O:19])(=[O:18])[CH2:8][O:7][C:6]=2[CH:20]=1.O.O.Cl[Sn]Cl.C([O-])([O-])=O.[Na+].[Na+]>C(OCC)(=O)C>[F:1][C:2]1[C:3]([NH2:21])=[CH:4][C:5]2[N:10]([CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[S:9](=[O:18])(=[O:19])[CH2:8][O:7][C:6]=2[CH:20]=1

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 61436Stannous chloride dihydrateHCID 54501274HCID 54501274, compound

Product 1

HCID 54067653HCID 54067653, compoundYield 67.2%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

A mixture of 6-fluoro-7-nitro-1-(phenylmethyl)-1H-4,2,1-benzoxathiazine 2,2-dioxide (1.96 g, 5.79 mmol) and SnCl2.2H2O (6.55 g, 29 mmol) in ethyl acetate (40 mL) was heated at reflux for 3 h. After the reaction was complete, ethyl acetate (400 mL) and then Na2CO3 (18.5 g) were added, and the mixture was stirred for 12 h. The resulting mixture was filtered and the filtrate was concentrated under reduced pressure to give 1.20 g of the title compound of Step G.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 3 h
  3. filtrationThe resulting mixture was filtered
  4. concentrationthe filtrate was concentrated under reduced pressure

Sources & evidence

ORD record
ord-3d701cda23ac4f8fa30b9c49c830d2ef
Source dataset
uspto-grants-1998_05
Patent number
US05750471

Reaction notes

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