4,4'-Dichlorobutyrophenone → HCID 13457142, Verbindung

HRID 462426

Reaktionsgleichung

Reaktionsgleichung von HRID 462426
Cl[CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)=[O:6].[Cl:14][C:15]1[CH:20]=[C:19]([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[CH:18]=[CH:17][C:16]=1[CH2:27][OH:28]>CC(C)=O.C(N(CC)CC)C>[Cl:13][C:10]1[CH:11]=[CH:12][C:7]([C:5](=[O:6])[CH2:4][CH2:3][CH2:2][N:24]2[CH2:23][CH2:22][N:21]([C:19]3[CH:18]=[CH:17][C:16]([CH2:27][OH:28])=[C:15]([Cl:14])[CH:20]=3)[CH2:26][CH2:25]2)=[CH:8][CH:9]=1

Komponenten

5

Edukt 2

HCID 27237814,4'-DichlorobutyrophenoneHCID 134571012-Chloro-4-(1-piperazinyl)benzenemethanol

Produkt 1

HCID 13457142HCID 13457142, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittel2×HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

A solution of 4,4'-dichlorobutyrophenone (4.5 g, 20.7 mmole) in 25 ml of acetone was added to a warm suspension of 2-chloro-4-(1-piperazinyl)benzenemethanol (4.7 g, 20.7 mole) in 50 ml acetone and 2.5 ml of triethylamine. The reaction mixture was refluxed for four days, cooled at -10° for three hours, and then filtered. The product was washed with a little acetone, triturated on the filter with water (four times, 50 ml), and air dried. Recrystallization from acetonitrile (65 ml) gave 3.0 g (35%), mp 137°-139°.

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for four days
  2. temperaturecooled at -10° for three hours
  3. filtrationfiltered
  4. washThe product was washed with a little acetone
  5. customtriturated on the
  6. filtrationfilter with water (four times, 50 ml), and air
  7. customdried
  8. customRecrystallization from acetonitrile (65 ml)
  9. customgave 3.0 g (35%), mp 137°-139°

Quellen und Nachweise

ORD-Eintrag
ord-cc769d2e0e8d40df8c844ef0c645c1d1
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04515793

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