Hydrochloric Acid → HCID 178433624, compound

HRID 1106522Notes

Reaction equation

HRID 1106522 reaction equation
[O:1]=[C:2]1[CH:6]([C:7](=[N:9][C:10]2[CH:14]=[CH:13][NH:12][N:11]=2)[CH3:8])[CH2:5][CH2:4][O:3]1.C(N(CC)CC)C.Cl.C(=O)([O-])O.[Na+]>O>[OH:3][CH2:4][CH2:5][C:6]1[C:2](=[O:1])[N:11]2[N:12]=[CH:13][CH:14]=[C:10]2[NH:9][C:7]=1[CH3:8]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 178463338HCID 178463338, compound

Product 1

HCID 178433624HCID 178433624, compoundYield 90.8%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
100 °C

Procedure

In 7.5 ml of water were suspended 1.17 g (6.04 mmol) of 3-{[1-(tetrahydro-2-oxo-3-furyl)ethylidene]amino}-pyrazole, and 0.73 g (7.23 mmol) of triethylamine were added to the suspension. The resultant mixture was stirred for 2 hours in an oil bath heated to 100° C. Thereafter, the reaction mixture was cooled with ice water, and concentrated hydrochloric acid was added thereto with stirring to adjust the pH of the reaction mixture to about 2 (deposit solids). Furthermore, a saturated aqueous solution of sodium hydrogencarbonate was added to adjust the pH of the mixture to about 4. Insoluble solids were collected by filtration, washed several times with water and air-dried to obtain 1.06 g (yield: 90.6%) of the intended product.

Workup

  1. additionwere added to the suspension
  2. additionwas added
  3. filtrationInsoluble solids were collected by filtration
  4. washwashed several times with water
  5. customair-dried

Sources & evidence

ORD record
ord-a184a78f72924388b4c0aa6b10f4d508
Source dataset
uspto-grants-2000_05
Patent number
US06057330

Reaction notes

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