Heptane → HCID 178443776, compound

HRID 2381872Notes

Reaction equation

HRID 2381872 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-a605caf4879c41e2a958fc6935d4f395
Source dataset
uspto-grants-2012_09
Patent number
US08258253B2

Reaction notes

Loading…