HCID 10751168, compound → HCID 67644432, compound

HRID 2210443Notes

Reaction equation

HRID 2210443 reaction equation
[CH:1]([NH:4][S:5]([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][C:13]=1[NH2:14])(=[O:7])=[O:6])([CH3:3])[CH3:2].[CH:15]([O-])([O-])OCC>>[CH:1]([N:4]1[CH:15]=[N:14][C:13]2[CH:12]=[CH:11][N:10]=[CH:9][C:8]=2[S:5]1(=[O:7])=[O:6])([CH3:3])[CH3:2]

Participants

3

Reactant 2

HCID 10751168HCID 10751168, compoundHCID 53630039Ethylorthoformate

Product 1

HCID 67644432HCID 67644432, compound

Conditions

Temperature
120 °C

Procedure

A mixture of 0.5 g of N-isopropyl-4- aminopyridine-3-sulfonamide (Preparation 7) and 5 cm3 of ethyl orthoformate is maintained in an open vessel at 120° C. for 4 hours. After concentrating the solution under partial vacuum, the oily residue obtained is triturated with 10 cm3 of ice-cold water. The crystalline precipitate which appears is collected on a filter and washed with water. It is recrystallized from a methanol/water (1/2) mixture.

Workup

  1. concentrationAfter concentrating the solution under partial vacuum
  2. customthe oily residue obtained
  3. customis triturated with 10 cm3 of ice-cold water
  4. customThe crystalline precipitate which appears is collected on
  5. filtrationa filter
  6. washwashed with water
  7. customIt is recrystallized from a methanol/water (1/2) mixture

Sources & evidence

ORD record
ord-bb7b227636a24786942a305742cc3497
Source dataset
uspto-grants-1995_10
Patent number
US05459138

Reaction notes

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