Hydrochloric Acid → HCID 86741652, compound

HRID 653448Notes

Reaction equation

HRID 653448 reaction equation
C([NH:4][CH:5]1[CH2:10][CH2:9][S:8](=[O:12])(=[O:11])[C:7]2[S:13][C:14]([S:16]([NH2:19])(=[O:18])=[O:17])=[CH:15][C:6]1=2)(=O)C.[ClH:20]>CO>[ClH:20].[NH2:4][C:5]1[CH2:10][CH2:9][S:8](=[O:12])(=[O:11])[CH:7]2[S:13][C:14]([S:16]([NH2:19])(=[O:18])=[O:17])=[CH:15][C:6]=12

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 13911597HCID 13911597, compound

Product 1

HCID 86741652HCID 86741652, compoundYield 79%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 5,6-dihydro-4-acetamido-4H-thieno[2,3-b]thiopyran-2-sulfonamide-7,7-dioxide, from Example 23, (2.0 g, 0.0062 mol) in CH3OH (20 ml) and 12N HCl (20 ml) was heated at reflux. After 6 hours, the solution was concentrated to dryness and the residue was treated with absolute ethanol. The mixture was concentrated to dryness and this procedure was repeated 4X. The final ethanol treatment was stirred, allowed to stand in the freezer overnight and filtered to yield 1.55 g (79%) of product; m.p. 251°-253° C.

Workup

  1. temperatureat reflux
  2. concentrationthe solution was concentrated to dryness
  3. additionthe residue was treated with absolute ethanol
  4. concentrationThe mixture was concentrated to dryness
  5. customto stand in the freezer overnight
  6. filtrationfiltered

Sources & evidence

ORD record
ord-2367ab9756cc488a8ba898995f1161b5
Source dataset
uspto-grants-1987_06
Patent number
US04677115

Reaction notes

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