Sodium Bicarbonate → HCID 178449047, compound

HRID 1158187Notes

Reaction equation

HRID 1158187 reaction equation
[PH2:1]([OH:3])=[O:2].[OH-].[CH2:5]([N+:9]([CH2:18][CH2:19][CH2:20][CH3:21])([CH2:14][CH2:15][CH2:16][CH3:17])[CH2:10][CH2:11][CH2:12][CH3:13])[CH2:6][CH2:7][CH3:8].C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1>[PH2:1]([O-:3])=[O:2].[CH2:18]([N+:9]([CH2:5][CH2:6][CH2:7][CH3:8])([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:14][CH2:15][CH2:16][CH3:17])[CH2:19][CH2:20][CH3:21]

Participants

5

Reactant 3

HCID 516892Sodium BicarbonateHCID 2723671Tetrabutylammonium HydroxideHCID 4124402Phosphinic Acid

Product 1

HCID 178449047HCID 178449047, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

A mixture of 50% aqueous hypophosphorous acid (6.6 g, 50 mmol) and toluene (30 mL) was cooled in ice and treated with tetrabutyl-ammonium hydroxide solution (32.4 g of 40% solution in water). The pH was adjusted to 7.00 by the addition of sodium bicarbonate. Toluene and the remaining water were removed under reduced pressure. The residue was dissolved in methyl ethyl ketone, filtered, and evaporated. The residue was triturated with diethyl ether and dried to afford a hygroscopic crystalline solid, 15.5 g.

Workup

  1. temperaturewas cooled in ice
  2. customToluene and the remaining water were removed under reduced pressure
  3. dissolutionThe residue was dissolved in methyl ethyl ketone
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was triturated with diethyl ether
  7. customdried
  8. customto afford a hygroscopic crystalline solid, 15.5 g

Sources & evidence

ORD record
ord-56bdef53090943489bde4b3c6b145568
Source dataset
uspto-grants-2010_10
Patent number
US07807755B2

Reaction notes

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