Bromine → HCID 53870913, compound

HRID 1112184Notes

Reaction equation

HRID 1112184 reaction equation
[CH:1]12[CH2:10][CH:6]([CH2:7][CH2:8][CH2:9]1)[CH:5]1[CH2:11][CH:2]2[CH2:3][CH2:4]1.[Br:12]Br.S([O-])(O)=O.[Na+]>>[Br:12][C:1]12[CH2:10][CH:6]([CH2:7][CH2:8][CH2:9]1)[CH:5]1[CH2:11][CH:2]2[CH2:3][CH2:4]1

Participants

4

Reactant 3

HCID 24408Bromine2×HCID 13070377HCID 13070377, compoundHCID 23665763Sodium Bisulfite

Product 1

HCID 53870913HCID 53870913, compound

Procedure

1.0 Gram (4.8 millimoles) of tricyclo [4.3.1.12,5 ] undecane is added to 2 ml (38.7 millimoles) of liquid bromine and the entirety is stirred at room temperature for 17 hours. The reaction mixture is added slowly to a cooled, saturated solution of sodium hydrogensulfite under stirring to decompose excess bromine. The aqueous solution is subjected to two extractions each with 20 ml of carbon tetrachloride and the combined extracts are dried with magnesium sulfate. Carbon tetrachloride is distilled out and the residue (1.9 g) is distilled under reduced pressure to collect a fraction boiling at 96°-8° C./2mmHg. Colorless crystals having a melting point of 57.5°-58.5° C. are thus obtained.

Workup

  1. stirringunder stirring
  2. extractionThe aqueous solution is subjected to two extractions each with 20 ml of carbon tetrachloride
  3. dry with materialthe combined extracts are dried with magnesium sulfate
  4. distillationCarbon tetrachloride is distilled out
  5. distillationthe residue (1.9 g) is distilled under reduced pressure
  6. customto collect a fraction boiling at 96°-8° C./2mmHg
  7. customare thus obtained

Sources & evidence

ORD record
ord-18b9926ab0264093b097e5db3045d77d
Source dataset
uspto-grants-1978_10
Patent number
US04120906

Reaction notes

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