Hydrochloric Acid → HCID 19786475, compound

HRID 1656906Notes

Reaction equation

HRID 1656906 reaction equation
[C:1]([NH:6][NH:7][C:8]([NH:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:9])([O:3]CC)=O.[OH-].[K+].Cl>O>[O:13]([CH2:12][CH2:11][N:10]1[C:1](=[O:3])[NH:6][NH:7][C:8]1=[O:9])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 15228776HCID 15228776, compound

Product 1

HCID 19786475HCID 19786475, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
95 °C

Procedure

The 1-(ethoxycarbonyl)semicarbazide VII (10.28 g, 0.0385 mol) was added to a solution of potassium hydroxide (4.96 g, 0.0769 mol) in water (105 mL) and the suspension was stirred and heated in an oil bath at 95° C. (oil bath temp.) for one hour. The yellow mixture was cooled to 25° C. and filtered. The filtrate was further cooled in an ice bath and neutralized by the slow addition of 6.72 ml (0.0807 mol) of conc. HCl. After 15 min. a white precipitate of VI was collected by filtration, washed with water and dried to constant weight. Yield: 6.56 g (77%); mp 187°-189° C. 1H NMR (DMSO-d6,): δ=10.15 (s, 2H, equivalent NH's).

Workup

  1. temperatureThe yellow mixture was cooled to 25° C.
  2. filtrationfiltered
  3. temperatureThe filtrate was further cooled in an ice bath
  4. filtrationAfter 15 min. a white precipitate of VI was collected by filtration
  5. washwashed with water
  6. customdried to constant weight

Sources & evidence

ORD record
ord-23719cae968f4bc9b7a5c935f5d32467
Source dataset
uspto-grants-1993_10
Patent number
US05256664

Reaction notes

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