Ammonium Chloride → 3-Fluoro-9-(1-methylpiperidin-4-yl)-9H-thioxanthen-9-ol

HRID 2083763Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2083763
[Mg].Cl[CH:3]1[CH2:8][CH2:7][N:6]([CH3:9])[CH2:5][CH2:4]1.[F:10][C:11]1[CH:12]=[CH:13][C:14]2[C:15](=[O:25])[C:16]3[C:21]([S:22][C:23]=2[CH:24]=1)=[CH:20][CH:19]=[CH:18][CH:17]=3.[Cl-].[NH4+]>O1CCCC1>[F:10][C:11]1[CH:12]=[CH:13][C:14]2[C:15]([CH:3]3[CH2:8][CH2:7][N:6]([CH3:9])[CH2:5][CH2:4]3)([OH:25])[C:16]3[C:21]([S:22][C:23]=2[CH:24]=1)=[CH:20][CH:19]=[CH:18][CH:17]=3

Komponenten

6

Edukt 4

HCID 25517Ammonium ChlorideHCID 793424-chloro-N-methylpiperidineHCID 5462224MagnesiumHCID 217304583-Fluoro-9H-thioxanthen-9-one

Produkt 1

HCID 203575253-Fluoro-9-(1-methylpiperidin-4-yl)-9H-thioxanthen-9-ol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

The Grignard reagent prepared from 0.62 g. of magnesium turnings and 3.5 g. of 4-chloro-N-methylpiperidine in tetrahydrofuran is treated with a solution of 3-fluoro-9-thioxanthone (3.0 g.) in 50 ml. of tetrahydrofuran. The mixture is refluxed for four hours, cooled, treated with saturated ammonium chloride solution and extracted with ether. The ether extract is washed with water, dried and concentrated to give 3-fluoro-9-(1-methyl-4-piperidyl)-thioxanthene-9-ol, m.p. 120°-130° C.

Aufarbeitung

  1. temperatureThe mixture is refluxed for four hours
  2. temperaturecooled
  3. extractionextracted with ether
  4. extractionThe ether extract
  5. washis washed with water
  6. customdried
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-ea2a40de98704208870f2e60807f27b1
Quelldatensatz
uspto-grants-1978_04
Patentnummer
US04086350

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