Hydrochloric Acid → HCID 20063614, compound

HRID 359639Notes

Reaction equation

HRID 359639 reaction equation
[NH2:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([N+:10]([O-:12])=[O:11])[C:5]([O:13][CH3:14])=[CH:4][C:3]=1[O:15][CH3:16].C(=O)([O-])[O-].[Ca+2].Cl[C:23]([O:25][CH2:26][CH2:27][Cl:28])=[O:24].Cl>O1CCOCC1.O>[Cl:28][CH2:27][CH2:26][O:25][C:23]([NH:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([N+:10]([O-:12])=[O:11])[C:5]([O:13][CH3:14])=[CH:4][C:3]=1[O:15][CH3:16])=[O:24]

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 10112Calcium CarbonateHCID 123052-Chloroethyl chloroformateHCID 23009735HCID 23009735, compound

Product 1

HCID 20063614HCID 20063614, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Conditions

Temperature
90 °C

Procedure

0.26 moles (60 g) of 2-amino-4-nitro-1,3,5-trimethoxybenzene are dissolved in 270 ml of dioxane. 26.3 g of calcium carbonate are added and the temperature is then raised to about 90° C. 0.34 moles (48.6 g) of chloroethyl chloroformate are then added with stirring. When the addition is complete, stirring is continued for additional 30 minutes at 90° C. The reaction mixture is diluted with 600 ml of iced water and is then acidified by adding 25 ml of concentrated hydrochloric acid. The precipitate obtained is filtered off and washed with water. After drying, it melts at 133° C.

Workup

  1. additionWhen the addition
  2. stirringstirring
  3. customThe precipitate obtained
  4. filtrationis filtered off
  5. washwashed with water
  6. customAfter drying

Sources & evidence

ORD record
ord-d71af70884674198a4244e8928149e1c
Source dataset
uspto-grants-1991_03
Patent number
US05002585

Reaction notes

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