Carbon Dioxide → HCID 19746918, compound

HRID 484266Notes

Reaction equation

HRID 484266 reaction equation
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([NH2:10])[C:5]=1[CH3:11])([O-:3])=[O:2].C(=O)([O-])[O-].[Ca+2].Cl[C:18]([O:20][CH2:21][CH2:22][Cl:23])=[O:19].C(=O)=O>O1CCOCC1.O>[CH3:11][C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=[CH:7][C:6]=1[NH:10][C:18](=[O:19])[O:20][CH2:21][CH2:22][Cl:23]

Participants

7

Reactant 4

HCID 280Carbon DioxideHCID 10112Calcium CarbonateHCID 117832-Methyl-3-nitroanilineHCID 123052-Chloroethyl chloroformate

Product 1

HCID 19746918HCID 19746918, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Conditions

Temperature
70 °C

Procedure

91 g of 2-nitro-6-aminotoluene and 31 g of calcium carbonate are initially introduced into the reaction vessel in 750 ml of dioxane, and are heated up to 70° C. 87 g of β-chloroethyl chloroformate are added dropwise to this mixture in the course of two hours such that the reaction mixture refluxes gently, carbon dioxide being evolved. The mixture is subsequently stirred under reflux for a further two hours and then cooled to 35° C., and water and ice are added. The product which has precipitated is filtered off with suction, washed with water, and dried.

Workup

  1. temperatureunder reflux for a further two hours
  2. temperaturecooled to 35° C.
  3. customThe product which has precipitated
  4. filtrationis filtered off with suction
  5. washwashed with water
  6. customdried

Sources & evidence

ORD record
ord-15d68ba2c5fe40cdbcd4830b68063836
Source dataset
uspto-grants-1993_07
Patent number
US05230710

Reaction notes

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