Water → HCID 20558416, compound

HRID 1659807Notes

Reaction equation

HRID 1659807 reaction equation
O.[CH2:2]([N:4]([CH2:20][CH3:21])[C:5]([CH2:7][NH:8][C:9]1[CH:14]=[C:13]([N+:15]([O-])=O)[CH:12]=[CH:11][C:10]=1[O:18][CH3:19])=[O:6])[CH3:3]>[Fe].C(O)(=O)C>[CH2:20]([N:4]([CH2:2][CH3:3])[C:5]([CH2:7][NH:8][C:9]1[CH:14]=[C:13]([NH2:15])[CH:12]=[CH:11][C:10]=1[O:18][CH3:19])=[O:6])[CH3:21]

Participants

5

Reactant 2

HCID 962WaterHCID 20558414HCID 20558414, compound

Product 1

HCID 20558416HCID 20558416, compound

Reagents, catalysts & solvents 2

HCID 23925IronCatalystHCID 176Acetic AcidSolvent

Conditions

Temperature
90 °C

Procedure

Into 120 ml of water, one adds 28 g of iron powder and 10 ml of acetic acid. The mixture is brought to a temperature of 85° C. under agitation. Then one adds, little by little, 0.1 mol (28 g) of 2-diethylcarbamylmethylamino-4-nitro anisole. The reaction medium is maintained for 10 minutes at a temperature of 90° C. Then one adds 14 ml of 10 N. soda solution. It is filtered boiling on a heated filter. By cooling the filtrate the expected product crystallizes. After recrystallization in water and vacuum drying it melts at 111° C.

Workup

  1. customis brought to a temperature of 85° C. under agitation
  2. additionThen one adds
  3. additionThen one adds 14 ml of 10 N
  4. filtrationIt is filtered
  5. filtrationfilter
  6. temperatureBy cooling the filtrate the expected product
  7. customcrystallizes
  8. customAfter recrystallization in water
  9. customvacuum drying it melts at 111° C.

Sources & evidence

ORD record
ord-56815a13b90e4ec9b5f0d601d94ee3a7
Source dataset
uspto-grants-1981_12
Patent number
US04305717

Reaction notes

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