Sodium Carbonate → 1,3-Dichloroisoquinoline

HRID 1006876

Reaktionsgleichung

Reaktionsgleichung von HRID 1006876
[C:1]1(=O)[NH:6][C:5](=O)[C:4]2=[CH:8][CH:9]=[CH:10][CH:11]=[C:3]2[CH2:2]1.[Cl-:13].[Cl-:14].C1(P(=O)([O-])[O-])C=CC=CC=1.C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:13][C:5]1[C:4]2[C:3](=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH:2]=[C:1]([Cl:14])[N:6]=1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 3494351,3(2H,4H)-isoquinolinedioneHCID 22048082HCID 22048082, Verbindung

Produkt 1

HCID 2986251,3-Dichloroisoquinoline

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture solution of homophthalimide (10.5 g) and phenylphosphonate dichloride (30 ml) was heated at 110° C. for 2 hr. After the reaction mixture was cooled, water was added thereto, and then the resulting mixture was neutralized with sodium carbonate. The resulting mixture was extracted with ethyl acetate, washed with brine, dried, and then the solvent was evaporated. The resulting residue was purified by silica gel column chromatography (methylene chloride), to give 9.30 g of the title compound as white crystals.

Aufarbeitung

  1. temperatureAfter the reaction mixture was cooled
  2. extractionThe resulting mixture was extracted with ethyl acetate
  3. washwashed with brine
  4. customdried
  5. customthe solvent was evaporated
  6. customThe resulting residue was purified by silica gel column chromatography (methylene chloride)

Quellen und Nachweise

ORD-Eintrag
ord-6979a33c740f4041a597c027f56fc455
Quelldatensatz
uspto-grants-2004_09
Patentnummer
US06790844B2

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