Calcium Carbonate → HCID 19878626, compound

HRID 1885500Notes

Reaction equation

HRID 1885500 reaction equation
[CH2:1]([O:8][C:9](Cl)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:12][NH:13][C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][C:15]=1[OH:23].C(=O)([O-])[O-].[Ca+2]>O1CCOCC1>[CH2:1]([O:8][C:9]([N:13]([C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][C:15]=1[OH:23])[CH3:12])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 10112Calcium CarbonateHCID 10387Benzyl chloroformateHCID 12306504HCID 12306504, compound

Product 1

HCID 19878626HCID 19878626, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

0.26 mole (40 ml) of benzylchloroformate are added dropwise to 0.24 mole (41.5 g) of 2-methylamino -5-nitrophenol and 15.6 g of calcium carbonate in 125 ml of dioxane brought to 80° C., the temperature being maintained at between 80° C. and 95° C. When the addition is complete, heating is maintained for a further 2 hours. The inorganic salts present in the reaction medium are removed by filtration while hot. After the addition of ice-cold water, the expected product crystallizes. The product obtained is recrystallized from acetic acid. It melts at 192° C.

Workup

  1. custombrought to 80° C.
  2. temperaturethe temperature being maintained at between 80° C. and 95° C
  3. additionWhen the addition
  4. temperatureheating
  5. temperatureis maintained for a further 2 hours
  6. customThe inorganic salts present in the reaction medium are removed by filtration while hot
  7. additionAfter the addition of ice-cold water
  8. customthe expected product crystallizes
  9. customThe product obtained
  10. customis recrystallized from acetic acid

Sources & evidence

ORD record
ord-9758358614354ea9a4203d4a8ca6785e
Source dataset
uspto-grants-1992_09
Patent number
US05145483

Reaction notes

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