Dichloromethane → 2-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine

HRID 350637

Reaktionsgleichung

Reaktionsgleichung von HRID 350637
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[CH2:5][CH2:6][N:7]=[C:8]1[N:13]=[CH:12][C:11]([CH3:15])([CH3:14])[CH2:10][S:9]1.[CH2:20]([N:22]([CH2:25]C)CC)[CH3:21].ClCCl.C(Cl)(=[S:34])OCC>O>[CH3:1][O:2][C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[CH2:5][CH2:6][N:7]=[C:8]1[N:13]([C:25](=[S:34])[NH:22][CH2:20][CH3:21])[CH2:12][C:11]([CH3:15])([CH3:14])[CH2:10][S:9]1

Komponenten

6

Edukt 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 5325481O-ethyl chloromethanethioateHCID 226399872-(2-Methoxyphenethyl)imino-5,5-dimethyl-1,3-thiazine

Produkt 1

HCID 226399822-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazineAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a mixture of 2-(2-methoxyphenethyl)imino-5,5-dimethyl-1,3-thiazine (0.28 g), triethylamine (0.15 g) and dichloromethane (5 ml) was added dropwise for 3 minutes ethyl chlorothiocarbonate (0.15 g). The mixture was stirred at room temperature for 2 hours. To the solution was added water (30 ml). The mixture was extracted with diethylether (60 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to give 2-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine (0.21 g, yield: 60%) as colorless oil.

Aufarbeitung

  1. extractionThe mixture was extracted with diethylether (60 ml)
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-7a469e139c884c078235231610693182
Quelldatensatz
uspto-grants-2007_02
Patentnummer
US07183275B2

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