Phosphorus sulfide (P2S5) → N-dodecylazepan-2-thione

HRID 981455

Reaktionsgleichung

Reaktionsgleichung von HRID 981455
[CH2:1]([N:13]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]1=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22]>C1C=CC=CC=1>[CH2:1]([N:13]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]1=[S:22])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

Komponenten

4

Edukt 2

HCID 14817Phosphorus sulfide (P2S5)HCID 42981Laurocapram

Produkt 1

HCID 10108679N-dodecylazepan-2-thioneAusbeute 40 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

To a solution of 5g (17.7mmol) of 1-n-dodecylazacycloheptan-2-one in 150ml of benzene was added 4.18g (9.4mmol) of phosphorus pentasulfide and the mixture was refluxed for 1 hr. After cooling to room temperature, the mixture was filtered and the solid was washed with chloroform and ethanol. The filtrate was concentrated in vacuo and the residue was subjected to flash chromatography, (silica; (95:5)V/V hexane/ethyl acetate) to give 2.11g (40%) of 1-n-dodecylazacycloheptane-2-thione.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 1 hr
  2. filtrationthe mixture was filtered
  3. washthe solid was washed with chloroform and ethanol
  4. concentrationThe filtrate was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d61690ac4ec3412db40a9f929e80f768
Quelldatensatz
uspto-grants-1991_02
Patentnummer
US04992422

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