Ammonia → HCID 178487562, compound

HRID 1154567Notes

Reaction equation

HRID 1154567 reaction equation
[C:1]([NH:4][C:5]([NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=1)=[O:6])(=O)[CH3:2].N>>[CH3:2][C:1]1[C:13]2[C:8](=[CH:9][C:10]([O:14][CH3:15])=[CH:11][CH:12]=2)[NH:7][C:5](=[O:6])[N:4]=1

Participants

3

Reactant 2

HCID 222AmmoniaHCID 13221147HCID 13221147, compound

Product 1

HCID 178487562HCID 178487562, compound

Conditions

Temperature
50 °C

Procedure

A mixture of 1-acetyl-3(3-methoxyphenyl)urea (32.5 g, 0.156 m) and polyphosphoric acid (912.5 g) is heated at 120°-130° C. for 2 hours. After cooling to 50° C. the melt is poured on ice-water (2 liters), and the solution is made weakly basic with ammonia and left standing overnight. The brownish-red precipitate which forms is filtered off, washed with cold water followed by hot acetone, and crystallized from ethanol (after treatment with charcoal) to give the product as a pale yellow solid; yield 11.5 g (39.1%); mp 251°-254° C.

Workup

  1. temperatureis heated at 120°-130° C. for 2 hours
  2. additionis poured on ice-water (2 liters)
  3. waitleft
  4. filtrationThe brownish-red precipitate which forms is filtered off
  5. washwashed with cold water
  6. customcrystallized from ethanol (after treatment with charcoal)

Sources & evidence

ORD record
ord-6b15bd1d8b67439793309e566e953e04
Source dataset
uspto-grants-1984_12
Patent number
US04490374

Reaction notes

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