HCID 131720540, compound → HCID 67639109, compound

HRID 863624Notes

Reaction equation

HRID 863624 reaction equation
C([C:5]1[N:6]([C:20](=[O:28])[C:21]2[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=2)[C:7]2[C:12]([C:13]=1[CH2:14][C:15]([O-:17])=[O:16])=[CH:11][CH:10]=[C:9]([O:18][CH3:19])[CH:8]=2)(C)(C)C>C1C=CC=CC=1>[Cl:27][C:24]1[CH:25]=[CH:26][C:21]([C:20]([N:6]2[C:7]3[C:12](=[CH:11][CH:10]=[C:9]([O:18][CH3:19])[CH:8]=3)[C:13]([CH2:14][C:15]([OH:17])=[O:16])=[CH:5]2)=[O:28])=[CH:22][CH:23]=1

Participants

3

Reactant 1

HCID 131720540HCID 131720540, compound

Product 1

HCID 67639109HCID 67639109, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Conditions

Temperature
210 °C

Procedure

A mixture of 1.0 g. of the ester obtained in step C and 0.1 powdered porous plate is heated, with stirring, in an oil bath at 210° C. under nitrogen, then dissolved in benzene and ether, filtered and extracted with sodium bicarbonate solution. The aqueous solution is filtered by suction to remove ether, neutralized with acetic acid, then acidified weakly with dilute hydrochloric acid. The crude product is then recrystallized from aqueous ethanol and dried in vacuo.

Workup

  1. additionA mixture of 1.0 g
  2. filtrationether, filtered
  3. extractionextracted with sodium bicarbonate solution
  4. filtrationThe aqueous solution is filtered by suction
  5. customto remove ether
  6. customThe crude product is then recrystallized from aqueous ethanol
  7. customdried in vacuo

Sources & evidence

ORD record
ord-b3e1c18a30914bfeb9c3620b1fa53f7e
Source dataset
uspto-grants-1998_02
Patent number
US05721347

Reaction notes

Loading…