Bromine → HCID 53870913, compound

HRID 1863242Notes

Reaction equation

HRID 1863242 reaction equation
[Br:1]Br.[CH:3]12[CH2:12][CH:8]([CH2:9][CH2:10][CH2:11]1)[CH:7]1[CH2:13][CH:4]2[CH2:5][CH2:6]1.S([O-])(O)=O.[Na+]>>[Br:1][C:3]12[CH2:12][CH:8]([CH2:9][CH2:10][CH2:11]1)[CH:7]1[CH2:13][CH:4]2[CH2:5][CH2:6]1

Participants

4

Procedure

To 20 ml (387 m mole) of liquid bromine was added 10 g (48 m mole) of tricyclo[4.3.1.12,5 ]undecane and the resulting mixture was stirred at room temperature for 17 hours. To a cooled saturated sodium hydrogen sulfite solution was added dropwise with stirring the reaction mixture to remove excess bromine. This aqueous solution was extracted twice with a portion of 200 ml of carbon tetrachloride, and the extract was dried over magnesium sulfate. The carbon tetrachloride was evaporated to obtain 19 g of the residue, which was distilled under reduced pressure, and the fraction having a boiling point of 96° to 98° C./2 mmHg was collected. This was a colorless crystalline material having a melting point of 57.5° to 58.5° C.

Workup

  1. stirringwith stirring the reaction mixture
  2. customto remove excess bromine
  3. extractionThis aqueous solution was extracted twice with a portion of 200 ml of carbon tetrachloride
  4. dry with materialthe extract was dried over magnesium sulfate
  5. customThe carbon tetrachloride was evaporated

Sources & evidence

ORD record
ord-531d2295d35141969576bfa86f3a3e5b
Source dataset
uspto-grants-1979_09
Patent number
US04168389

Reaction notes

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