Phosphorus tribromide → HCID 10560066, compound

HRID 1975312Notes

Reaction equation

HRID 1975312 reaction equation
P(Br)(Br)[Br:2].[CH:5]1([CH:8]([CH:12]2[CH2:14][CH2:13]2)[CH2:9][CH2:10]O)[CH2:7][CH2:6]1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>CCOCC>[Br:2][CH2:10][CH2:9][CH:8]([CH:12]1[CH2:14][CH2:13]1)[CH:5]1[CH2:7][CH2:6]1

Participants

5

Reactant 3

HCID 24614Phosphorus tribromideHCID 10820614HCID 10820614, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 10560066HCID 10560066, compoundYield 60%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

15.5 g of phosphorus tribromide are slowly added to a solution, cooled to -30° C., of 22 g of 3,3-dicyclopropylpropanol (obtained by reduction of the compound described in preparation A in the presence of lithium aluminum hydride) in 85 ml of anhydrous ether, and the mixture is poured, after returning to room temperature, into 7 ml of ice cold water. The organic phase is then washed with a saturated solution of sodium bicarbonate and then with water until neutral and finally dried and evaporated. The expected product is obtained after distillation under vacuum.

Workup

  1. customobtained by reduction of the compound
  2. additionthe mixture is poured
  3. washThe organic phase is then washed with a saturated solution of sodium bicarbonate
  4. dry with materialwith water until neutral and finally dried
  5. customevaporated

Sources & evidence

ORD record
ord-3c9ac55131d945abb8507b2453c9071f
Source dataset
uspto-grants-1994_02
Patent number
US05286732

Reaction notes

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