Formic Acid → HCID 14456844, compound

HRID 1649768Notes

Reaction equation

HRID 1649768 reaction equation
[CH:1]([OH:3])=O.C(OC(=O)C)(=O)C.[NH2:11][CH2:12][CH2:13][S:14][C:15]1[CH:16]=[CH:17][C:18]2[N:19]([CH:21]=[CH:22][N:23]=2)[N:20]=1>O1CCCC1>[CH:1]([NH:11][CH2:12][CH2:13][S:14][C:15]1[CH:16]=[CH:17][C:18]2[N:19]([CH:21]=[CH:22][N:23]=2)[N:20]=1)=[O:3]

Participants

5

Reactant 3

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 19854390HCID 19854390, compound

Product 1

HCID 14456844HCID 14456844, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

On the other hand, 5.52 g of formic acid is added to 12.25 g of acetic anhydride at room temperature and the mixture is stirred at 45°-50° C. for 1 hour. After cooling, 60 ml of tetrahydrofuran and 5.83 g of the above-prepared crystals of 6-(2-aminoethylthio)imidazo[1,2-b]pyridazine are added and the mixture is stirred at room temperature for 1 hour. The solvent is distilled off under reduced pressure and the residue made basic with a saturated aqueous solution of sodium hydrogen carbonate. The precipitated crystals are collected by filtration to give 2.83 g of 6-(2-formylaminoethylthio)imidazo[1,2-b]pyridazine as colorless crystals melting at 148° to 151° C.

Workup

  1. temperatureAfter cooling
  2. stirringthe mixture is stirred at room temperature for 1 hour
  3. distillationThe solvent is distilled off under reduced pressure
  4. filtrationThe precipitated crystals are collected by filtration

Sources & evidence

ORD record
ord-aeea2949822c4c6999d04bb31596ac29
Source dataset
uspto-grants-1990_05
Patent number
US04921851

Reaction notes

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