Nitric Acid → HCID 13279117, compound

HRID 1388683Notes

Reaction equation

HRID 1388683 reaction equation
[Cl:1][CH2:2][CH:3]1[O:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[O:5][CH2:4]1.[N+:13]([O-])([OH:15])=[O:14]>C(O)(=O)C.O>[Cl:1][CH2:2][CH:3]1[O:8][C:7]2[CH:9]=[C:10]([N+:13]([O-:15])=[O:14])[CH:11]=[CH:12][C:6]=2[O:5][CH2:4]1

Participants

5

Reactant 2

HCID 944Nitric AcidHCID 953202-(Chloromethyl)-2,3-dihydro-1,4-benzodioxin

Product 1

HCID 13279117HCID 13279117, compound

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolvent2×HCID 962WaterSolvent

Procedure

92 g of 2-chloromethyl 2,3-dihydro [4H] 1,4-benzodioxin are dissolved in 675 ml acetic acid. In this solution it is added a mixture of 500 ml acetic acid and 250 ml nitric acid while keeping the temperature below 20°. The mixture is kept at room temperature for 2 hours then heated at 90° for 1 hour. It is thereafter poured in water and extracted with methylene chloride. 102 g of the nitroderivative are obtained. It is in the form of yellow crystalls which melt at 60°-62°.

Workup

  1. additionIn this solution it is added
  2. customthe temperature below 20°
  3. temperaturethen heated at 90° for 1 hour
  4. extractionextracted with methylene chloride
  5. custom102 g of the nitroderivative are obtained
  6. custommelt at 60°-62°

Sources & evidence

ORD record
ord-93a38a6f5745400b81622dc0f58dae39
Source dataset
uspto-grants-1984_02
Patent number
US04432984

Reaction notes

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