Diisopropylamine → N,N-Diisopropyl-1,3,2-oxathiaphospholan-2-amine

HRID 1081557Notes

Reaction equation

HRID 1081557 reaction equation
Cl[P:2]1[S:6][CH2:5][CH2:4][O:3]1.[CH:7]([NH:10][CH:11]([CH3:13])[CH3:12])([CH3:9])[CH3:8]>CCCCC>[CH:7]([N:10]([P:2]1[S:6][CH2:5][CH2:4][O:3]1)[CH:11]([CH3:13])[CH3:12])([CH3:9])[CH3:8]

Participants

4

Reactant 2

HCID 7912DiisopropylamineHCID 111943992-Chloro-1,3,2-oxathiaphospholane

Product 1

HCID 15276683N,N-Diisopropyl-1,3,2-oxathiaphospholan-2-amine

Reagents, catalysts & solvents 1

HCID 8003PentaneSolvent

Procedure

Compound 1 (0.2 mol) is dissolved in n-pentane (300 mL) and diisopropylamine (0.4 mol) is added dropwise. The reaction mixture is stirred at room temperature for 30 minutes, after which diisopropylamine hydrochloride is filtered off, solvent is evaporated under reduced pressure and crude product is purified by vacuum distillation. Product 2 is obtained as the fraction boiling at 70° C./0.1 mm Hg and is characterized by 31P NMR and mass spectroscopy.

Workup

  1. filtrationafter which diisopropylamine hydrochloride is filtered off
  2. customsolvent is evaporated under reduced pressure and crude product
  3. distillationis purified by vacuum distillation

Sources & evidence

ORD record
ord-d8b8903d3fa243f8954e9f68a8f9035e
Source dataset
uspto-grants-1996_12
Patent number
US05587361

Reaction notes

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