Calcium Carbonate → HCID 14453738, compound

HRID 1721165Notes

Reaction equation

HRID 1721165 reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.C(=O)([O-])[O-].[Ca+2].Cl[C:19]([O:21][CH2:22][CH2:23][Cl:24])=[O:20]>COCCOCCOC.O>[Cl:24][CH2:23][CH2:22][O:21][C:19](=[O:20])[NH:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1

Participants

6

Reactant 3

HCID 10112Calcium CarbonateHCID 123052-Chloroethyl chloroformateHCID 123071Benzenamine, 4-methoxy-3-nitro-

Product 1

HCID 14453738HCID 14453738, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolvent2×HCID 8150DiglymeSolvent

Conditions

Temperature
78 °C

Procedure

420.5 g of 4-amino-2-nitroanisole are dissolved in 1275 ml of diethylene glycol dimethyl ether and 150 ml of water, 135 g of calcium carbonate are added and the mixture is heated to 78° C. 375 g of 2-chloroethyl chloroformate are allowed to run into this mixture in the course of 3 hours such that the reaction temperature remains at 78°-80° C. The mixture is subsequently stirred for 1.5 hours to bring the reaction to completion and is cooled to 35° C. and water and ice are added. The product which has precipitated is filtered off, washed with water and dried.

Workup

  1. customto run into this mixture in the course of 3 hours such that the reaction temperature
  2. customremains at 78°-80° C
  3. customthe reaction to completion
  4. temperatureis cooled to 35° C.
  5. customThe product which has precipitated
  6. filtrationis filtered off
  7. washwashed with water
  8. customdried

Sources & evidence

ORD record
ord-f6b05e8af433465e9293dbb2dd309b2f
Source dataset
uspto-grants-1996_04
Patent number
US05508467

Reaction notes

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