Azane;hydrate → HCID 13329100, compound

HRID 2351238Notes

Reaction equation

HRID 2351238 reaction equation
Cl[S:2]([C:5]1[N:9]([CH3:10])[N:8]=[C:7]([CH3:11])[C:6]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])(=[O:4])=[O:3].O.[NH3:18]>C1COCC1>[NH2:18][S:2]([C:5]1[N:9]([CH3:10])[N:8]=[C:7]([CH3:11])[C:6]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])(=[O:4])=[O:3]

Participants

4

Reactant 2

HCID 12896473Azane;hydrateHCID 13329096HCID 13329096, compound

Product 1

HCID 13329100HCID 13329100, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

4.6 g of ethyl 5-chlorosulfonyl-1,3-dimethylpyrazole-4-carboxylate is dissolved in 8 ml of THF, and the solution is added dropwise to 25 ml of ammonia water at 5° C. to 7° C. The reaction mixture is stirred at the same temperature for 1 hour, and then concentrated to dryness under reduced pressure. To the residue is added ethyl acetate, followed by filtration to remove impurities, and the filtrate is concentrated under reduced pressure. The residue is diluted with n-hexane, and then cooled with ice to give crystals. The crystals are filtered and dried to yield 3.6 g of the title compound. mp. 112° to 113° C.

Workup

  1. concentrationconcentrated to dryness under reduced pressure
  2. additionTo the residue is added ethyl acetate
  3. filtrationfollowed by filtration
  4. customto remove impurities
  5. concentrationthe filtrate is concentrated under reduced pressure
  6. additionThe residue is diluted with n-hexane
  7. temperaturecooled with ice
  8. customto give crystals
  9. filtrationThe crystals are filtered
  10. customdried

Sources & evidence

ORD record
ord-78a8b215f1114c3e8989f22f9964133a
Source dataset
uspto-grants-1989_10
Patent number
US04872901

Reaction notes

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