2,4,6-Trimethylpyridine → HCID 22644528, compound

HRID 2414237Notes

Reaction equation

HRID 2414237 reaction equation
C([O:3][P:4]([CH2:9][O:10][CH2:11][CH2:12][NH:13][OH:14])(=[O:8])[O:5]CC)C.N1C(C)=CC(C)=CC=1C>C(Cl)Cl>[OH:14][NH:13][CH2:12][CH2:11][O:10][CH2:9][P:4](=[O:3])([OH:8])[OH:5]

Participants

4

Reactant 2

HCID 79532,4,6-TrimethylpyridineHCID 73948924HCID 73948924, compound

Product 1

HCID 22644528HCID 22644528, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
100 °C

Procedure

With reference to K -L. Yu, J. J.Bronson, H.Yang, A.Patick, M.Alam, V.Brankovan, R.Datema, M. J. M.Hitchcock, J. C.Martin, J. Med. Chem. 1992, 35, 2958-2969 0.5 mol [2-(N-hydroxyamino)-ethoxy]methylphosphonic acid diethylester and 1 mol 2,4,6-collidine in 5 ml of absolute methylenechloride are stirred under argon for one hour at a temperature of 0° C. After allowing to stand for 16 hours at room temperature the-solution is concentrated in vacuum, taken up in watery acetone and stirred for 14 hours. Subsequently it is taken up in 1 n NaOH and heated to 100° C. for 2 h. After cooling-off it is concentrated and the raw product purified by chromatography.

Workup

  1. concentrationthe-solution is concentrated in vacuum
  2. concentrationAfter cooling-off it is concentrated
  3. customthe raw product purified by chromatography

Sources & evidence

ORD record
ord-085b453bee26445681896f5d3f9a2729
Source dataset
uspto-grants-2004_11
Patent number
US06812224B2

Reaction notes

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