HCID 70358042, compound → HCID 15718652, compound

HRID 2165367Notes

Reaction equation

HRID 2165367 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:16]3[C:11](=[N:12][CH:13]=[CH:14][CH:15]=3)[N:10](C)[C:9]=2C=CC(O)CC(O)CC(OCC)=O)=[CH:4][CH:3]=1>C(O)COCCO>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:16]3[C:11](=[N:12][CH:13]=[CH:14][CH:15]=3)[NH:10][CH:9]=2)=[CH:6][CH:7]=1

Participants

3

Reactant 1

HCID 70358042HCID 70358042, compound

Product 1

HCID 15718652HCID 15718652, compound

Reagents, catalysts & solvents 1

HCID 8117Diethylene GlycolSolvent

Procedure

In a vessel, under nitrogen, about 27 g of the crude product of Step 1, above, in about 300 ml of diethylene glycol is refluxed (at about 250°) for about 7 hours. The contents are cooled, and then quenched with water yielding a yellow precipitate. The precipitate is washed thoroughly with water, then once with petroleum ether. The product is dissolved in ethyl acetate, dried and then concentrated by evaporation until precipitation begins. The precipitate is recovered by filtration, and washed first with cold ethyl acetate, then with petroleum ether yielding the title product of this step as yellow solids (mp 190°-192°).

Workup

  1. temperatureThe contents are cooled
  2. customquenched with water yielding a yellow precipitate
  3. washThe precipitate is washed thoroughly with water
  4. dissolutionThe product is dissolved in ethyl acetate
  5. customdried
  6. concentrationconcentrated by evaporation until precipitation
  7. filtrationThe precipitate is recovered by filtration
  8. washwashed first with cold ethyl acetate

Sources & evidence

ORD record
ord-23ddfb3bc3294e2c8b4a5070eca2a542
Source dataset
uspto-grants-1990_07
Patent number
US04939159

Reaction notes

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