Heptane → HCID 178443776, compound

HRID 2090112Notes

Reaction equation

HRID 2090112 reaction equation
[CH2:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH:2]=[CH2:3].[PH2:13]([OH:15])=[O:14].C1C(C(OOC(C)(C)C)=O)=CC=CC=1.CCCCCCC>C(O)(C)C.O>[CH2:5]([O:4][CH2:1][CH2:2][CH2:3][PH:13](=[O:14])[OH:15])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

Participants

7

Reactant 4

HCID 8900HeptaneHCID 11966tert-Butyl peroxybenzoateHCID 520600Allyl octyl etherHCID 4124402Phosphinic Acid

Product 1

HCID 178443776HCID 178443776, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 3776IsopropanolSolvent

Procedure

Allyloxyoctane of step a) (15 g, 0.0882 mols), 50% hypophosphorous acid (15 mL, 0.0882 mols) and tert-butyl perbenzoate (1 mL) in 100 mL isopropyl alcohol are heated at 100° C. for 26 hrs. After completion of the reaction, a mixture of 200 mL n-heptane and water (1:1) is added and the mixture is stirred for 30 minutes. The organic phase is separated and is washed with water. It is dried over Na2SO4 and concentrated to give 16.2 g of oily product. The characterization of the crude material by 1H and 31P NMR shows the formation of product with 63% purity.

Workup

  1. customAfter completion of the reaction
  2. additionis added
  3. customThe organic phase is separated
  4. washis washed with water
  5. dry with materialIt is dried over Na2SO4
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-b29a7ac0be75495cb067c2628ca628cb
Source dataset
uspto-grants-2013_05
Patent number
US08436131B2

Reaction notes

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