HCID 836063, compound → HCID 11805638, compound

HRID 1461794Notes

Reaction equation

HRID 1461794 reaction equation
[C:1]([NH:9][C:10]1[C:11](Cl)=[N:12][CH:13]=[CH:14][CH:15]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[Si](OP(=O)=O)(C)C>>[C:2]1([C:1]2[O:8][C:11]3[C:10]([N:9]=2)=[CH:15][CH:14]=[CH:13][N:12]=3)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

3

Reactant 2

HCID 836063HCID 836063, compoundHCID 16133246Trimethyl(phosphooxy)silane

Product 1

HCID 11805638HCID 11805638, compound

Procedure

1.9 g (8 mmol) of 3-benzoylamino-2-chloropyridine, prepared in stage A, are added to the PPSE solution and then brought to reflux for 15 hours. The 1,2-dichlorobenzene is then evaporated off under vacuum. The residue is treated with a water/ice mixture. The pH of the solution is adjusted to 7-8 with 5% sodium bicarbonate solution. The precipitated product is filtered off and then recrystallized in cyclohexane.

Workup

  1. temperatureto reflux for 15 hours
  2. customThe 1,2-dichlorobenzene is then evaporated off under vacuum
  3. additionThe residue is treated with a water/ice mixture
  4. filtrationThe precipitated product is filtered off
  5. customrecrystallized in cyclohexane

Sources & evidence

ORD record
ord-0933c67cb8884196afc3fb36c86ef009
Source dataset
uspto-grants-1991_12
Patent number
US05077408

Reaction notes

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