Water → Methyl 1-methyl-N-[(methylsulphonyl)acetyl]-2-(phenylmethylene)hydrazinecarboximidothioate

HRID 652090Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 652090
Cl.[CH3:2][N:3]([C:12]([S:14][CH3:15])=[NH:13])[N:4]=[CH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(N(CC)CC)C.[CH3:23][S:24]([CH2:27][C:28](Cl)=[O:29])(=[O:26])=[O:25].O>ClCCl>[CH3:2][N:3]([C:12]([S:14][CH3:15])=[N:13][C:28](=[O:29])[CH2:27][S:24]([CH3:23])(=[O:26])=[O:25])[N:4]=[CH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 21288095(Methanesulfonyl)acetyl chlorideHCID 70434230HCID 70434230, Verbindung

Produkt 1

HCID 70434558Methyl 1-methyl-N-[(methylsulphonyl)acetyl]-2-(phenylmethylene)hydrazinecarboximidothioateAusbeute 35,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a stirred solution of methyl 1-methyl-2-(phenylmethylene)hydrazinecarboximidothioate hydrochloride (5.71 g) and triethylamine (5.2 g) in dichloromethane (100 ml) was added methylsulphonylacetyl chloride (4.9 g) in dichloromethane (20 ml) dropwise during 0.5 h at 20°. The mixture was stirred at 20° during 18 h, water (100 ml) added and the phase separated. The dichloromethane layer was washed with water, dried, and evaporated. The residue was crystallised from ethanol to give the title compound (2.7 g) as off white needles. m.p. 149.5°-150.5°.

Aufarbeitung

  1. customthe phase separated
  2. washThe dichloromethane layer was washed with water
  3. customdried
  4. customevaporated
  5. customThe residue was crystallised from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-49cb13b3f12a437d9dd3ede10a39b81f
Quelldatensatz
uspto-grants-1987_06
Patentnummer
US04670448

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