HCID 21568305, compound → HCID 21568302, compound

HRID 1579308Notes

Reaction equation

HRID 1579308 reaction equation
[CH2:1]([P:3]1(=[O:13])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6][CH2:5][CH2:4]1)C>O1CCCC1>[CH2:4]([P:3]1(=[O:13])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:1]1)[CH3:5]

Participants

3

Reactant 1

HCID 21568305HCID 21568305, compound

Product 1

HCID 21568302HCID 21568302, compoundYield 72%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

This compound was prepared from 1-hydroxy-phosphindoline 1-oxide (3.0g, 17.9 mmol) by a method similar to that used for the preparation of 1-ethyl-1,2,3,4-tetrahydrophosphinoline 1-oxide described above, except that anhydrous tetrahydrofuran was used as solvent. Isolation with chloroform and bulb to bulb distillation of the residue at 160°/0,1 mm gave a colourless hygroscopic liquid (2.3 g, 72%). Preparative T.l.c. (RF 0.38, chloroform/methanol 15:1), and bulb to bulb distillation of the major component gave "pure" 1-ethylphosphindoline-1-oxide as a colourless hygroscopic liquid. This was shown to be pure by g.l.c.

Workup

  1. distillationIsolation with chloroform and bulb to bulb distillation of the residue at 160°/0,1 mm

Sources & evidence

ORD record
ord-6891720415e04866bf211691a33a3f0e
Source dataset
uspto-grants-1976_01
Patent number
US03931196

Reaction notes

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