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

HRID 53503Notes

Reaction equation

HRID 53503 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 dhisopropylamine 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 arid mass spectroscopy.

Workup

  1. filtrationafter which dhisopropylamine 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-a24eb1a7d7e74b688d316ba4012c38f4
Source dataset
uspto-grants-1997_04
Patent number
US05620963

Reaction notes

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