Hydrochloric Acid → HCID 178433624, compound

HRID 1586046Notes

Reaction equation

HRID 1586046 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-ae65c32f7be94e5680579333db9a6f87
Source dataset
uspto-grants-1999_08
Patent number
US05942515

Reaction notes

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