Diethylamine → HCID 54132934, compound

HRID 1855955Notes

Reaction equation

HRID 1855955 reaction equation
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[Cl:6][C:7]([PH:15]([C:17]1(Cl)[CH:22]=[CH:21][CH:20]=[CH:19][CH2:18]1)=[O:16])([Cl:14])[C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9]>C(OCC)C.C(Cl)CCC>[Cl:14][C:7]([P:15]([N:3]([CH2:4][CH3:5])[CH2:1][CH3:2])([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:16])([Cl:6])[C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9]

Participants

5

Reactant 2

HCID 8021DiethylamineHCID 178459573HCID 178459573, compound

Product 1

HCID 54132934HCID 54132934, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolvent2×HCID 8005Butyl ChlorideSolvent

Procedure

A solution of 11.7 g of diethylamine in 100 ml of diethylether is added dropwise to a solution of 27.1 g of 1-methylethyl 2,2-dichloro-[(1-chloro)phenylphosphinyl]-acetate in 200 ml of ether at 0°. After stirring at room temperature for 1 hour, the solution is washed with water and with 10% sodium bicarbonate solution, then dried over MgSO4 and stripped to give a dark oil. The reaction product is dissolved in n-butyl chloride, washed with water, contacted with activated carbon, dried over MgSO4 and stripped to give substantially pure 1-methylethyl 2,2-dichloro-[(diethylamino)phenylphosphinyl]acetate.

Workup

  1. washthe solution is washed with water and with 10% sodium bicarbonate solution
  2. dry with materialdried over MgSO4
  3. customto give a dark oil
  4. washwashed with water
  5. dry with materialdried over MgSO4

Sources & evidence

ORD record
ord-4c54fdd4f20140219718a952af916576
Source dataset
uspto-grants-1980_08
Patent number
US04217312

Reaction notes

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