Acetic Anhydride → HCID 10633310, compound

HRID 2210451Notes

Reaction equation

HRID 2210451 reaction equation
[NH2:1][C:2]1[C:7]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:6][C:5]([Cl:12])=[CH:4][N:3]=1.[C:13](OC(=O)C)(=O)[CH3:14]>>[Cl:12][C:5]1[CH:4]=[N:3][C:2]2[NH:1][C:13]([CH3:14])=[N:11][S:8](=[O:9])(=[O:10])[C:7]=2[CH:6]=1

Participants

3

Reactant 2

HCID 7918Acetic AnhydrideHCID 27796732-amino-5-chloropyridine-3-sulfonamide

Product 1

HCID 10633310HCID 10633310, compound

Procedure

A mixture of 1 g of 2-amino-5-chloropyridine-3- sulfonamide (Preparation 20) and 10 cm3 of acetic anhydride is brought to reflux for 6 hours. After cooling, the crystals are filtered off, washed with a small amount of acetic anhydride and then with diethyl ether and dried. The crystals are redissolved in 50 cm3 of 0.1N NaOH. The possible insoluble material is removed by filtration. The filtrate, adjusted to a pH of 4 using formic acid, allows crystals to precipitate. They are collected on a filter, washed with water and dried.

Workup

  1. temperatureto reflux for 6 hours
  2. temperatureAfter cooling
  3. filtrationthe crystals are filtered off
  4. washwashed with a small amount of acetic anhydride
  5. dry with materialwith diethyl ether and dried
  6. dissolutionThe crystals are redissolved in 50 cm3 of 0.1N NaOH
  7. customThe possible insoluble material is removed by filtration
  8. customto precipitate
  9. customThey are collected on a filter
  10. washwashed with water
  11. customdried

Sources & evidence

ORD record
ord-c361a3ef5cf040938c8c96b9710db92f
Source dataset
uspto-grants-1995_10
Patent number
US05459138

Reaction notes

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