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Potassium Iodide → N-butyl-3,3-bis(diethoxyphosphinyl)propionamide

HRID 1972
Notes
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Reaction equation

HRID 1972 reaction equation
[CH2:1]([P:10](=[O:17])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])[P:2](=[O:9])([O:6][CH2:7][CH3:8])[O:3][CH2:4][CH3:5].[H-].[Na+].[H-].[CH2:21]([NH:25][C:26](=[O:29])[CH2:27]Cl)[CH2:22][CH2:23][CH3:24].[I-].[K+].[Cl-].[Na+]>C1COCC1>[CH2:21]([NH:25][C:26](=[O:29])[CH2:27][CH:1]([P:2]([O:6][CH2:7][CH3:8])([O:3][CH2:4][CH3:5])=[O:9])[P:10]([O:11][CH2:12][CH3:13])([O:14][CH2:15][CH3:16])=[O:17])[CH2:22][CH2:23][CH3:24]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 6

HCID 4875Potassium IodideHCID 5234Sodium ChlorideHCID 15455Tetraethyl methylenediphosphonateHCID 24758Sodium hydrideHCID 166653HydrideHCID 219645N-butyl-2-chloroacetamide

Product 1

HCID 19689044
N-butyl-3,3-bis(diethoxyphosphinyl)propionamide
Yield 70%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent3×

Procedure

Tetraethyl methylenebisphosphonate (1.44 g, 5.0 mmol) in THF (1 mL) was added to a slurry of 80% sodium hydride (150 mg, 5.0 mmol) in THF (4 mL) at 0° C. The reaction was warmed to room temperature and stirred until all of the hydride was consumed. A solution of N-butyl-2-chloroacetamide (0.75 g, 5.0 mmol) in THF (1 ml) and potassium iodide (100 mg) were then added. The reaction mixture was then heated at 50° C. for 18 hours, during which time sodium chloride precipitated. Additional sodium hydride (20 mg) was added, and the reaction mixture was heated an additional 4 hours. After cooling, the mixture was poured into 1N HCl (10 mL) and diethyl ether (50 mL) was added. The diethyl ether layer was further extracted with water (3×10 mL). The combined aqueous fractions were extracted with dichloromethane (4×25 mL). The combined extracts were dried (Na2SO4) and concentrated to give the title compound (1.40 g, 70%) as an oil.

Workup

  1. customwas consumed
  2. customprecipitated
  3. additionAdditional sodium hydride (20 mg) was added
  4. temperaturethe reaction mixture was heated an additional 4 hours
  5. temperatureAfter cooling
  6. additionthe mixture was poured into 1N HCl (10 mL) and diethyl ether (50 mL)
  7. additionwas added
  8. extractionThe diethyl ether layer was further extracted with water (3×10 mL)
  9. extractionThe combined aqueous fractions were extracted with dichloromethane (4×25 mL)
  10. dry with materialThe combined extracts were dried (Na2SO4)
  11. concentrationconcentrated

Sources & evidence

ORD record
ord-0d06fa7cb400433aac9523d5cb4e75c0
Source dataset
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05728650

Reaction notes

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