Hydrochloric Acid → HCID 14405129, compound

HRID 476978Notes

Reaction equation

HRID 476978 reaction equation
Br[CH2:2][C:3]1[CH:15]=[CH:14][C:6]2[O:7][C:8]([F:13])([F:12])[CH:9]([F:11])[O:10][C:5]=2[CH:4]=1.C1N2CN3CN(C2)CN1C3.Cl.[OH2:27]>>[CH:2]([C:3]1[CH:15]=[CH:14][C:6]2[O:7][C:8]([F:13])([F:12])[CH:9]([F:11])[O:10][C:5]=2[CH:4]=1)=[O:27]

Participants

5

Reactant 4

HCID 313Hydrochloric AcidHCID 962Water2×HCID 4101HexamethylenetetramineHCID 14405128HCID 14405128, compound

Product 1

HCID 14405129HCID 14405129, compound

Procedure

318 g of 6-bromomethyl-2,2,3-trifluoro-1,4-benzodioxane are added to 318 g of urotropin in 630 ml of water, the reaction mixture is heated under reflux for 2 hours, 318 ml of hydrochloric acid and 470 ml of water are then added and the mixture is heated for a further 3 hours. The product is driven over with steam and is separated off and, after drying, distilled. 158 g of distillate are obtained (boiling point: 112-115° C. (under 18 mbar)) and partly crystallize on standing. The crystal sludge is filtered off with suction and the crystals are washed with cold petroleum ether.

Workup

  1. temperaturethe reaction mixture is heated
  2. temperatureunder reflux for 2 hours
  3. temperaturethe mixture is heated for a further 3 hours
  4. customis separated off
  5. customafter drying
  6. distillationdistilled
  7. custom158 g of distillate are obtained (boiling point: 112-115° C. (under 18 mbar))
  8. custompartly crystallize
  9. filtrationThe crystal sludge is filtered off with suction
  10. washthe crystals are washed with cold petroleum ether

Sources & evidence

ORD record
ord-b0205274e7324ef081ce1d391e9f252e
Source dataset
uspto-grants-1989_12
Patent number
US04886816

Reaction notes

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