3-Chlorotoluene → HCID 178443608, Verbindung

HRID 481966

Reaktionsgleichung

Reaktionsgleichung von HRID 481966
O.CS[C:4]1[NH:9][C:8]2[CH:10]=[CH:11][N:12]=[CH:13][C:7]=2[S:6](=[O:15])(=[O:14])[N:5]=1.[CH2:16]([NH2:24])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23].ClC1C=C(C)C=CC=1>>[CH2:16]([NH:24][C:4]1[NH:9][C:8]2[CH:10]=[CH:11][N:12]=[CH:13][C:7]=2[S:6](=[O:15])(=[O:14])[N:5]=1)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23]

Komponenten

4

Edukt 3

HCID 79313-ChlorotolueneHCID 8143OctylamineHCID 190647513-Methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate

Produkt 1

HCID 178443608HCID 178443608, Verbindung

Versuchsvorschrift

A mixture of 3-methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate (0.5 g), octylamine (0.5 mL) and m-chlorotoluene (3 mL) was refluxed for 2-3 h (until completion of the reaction; t.l.c.). Most of the solvents were removed by distillation and the residue was dispersed in a mixture of water (30 mL) and methanol (30 mL) and supplemented with NaOH 10% w/v in water (2 mL). The mixture was treated with charcoal, filtered, and the filtrate was adjusted to pH 6 with 1N HCl. The resulting precipitate was collected by filtration, washed with water and dried (yield: 0.29 g); m.p. 176°-179° C. (Compound 13).

Aufarbeitung

  1. temperaturewas refluxed for 2-3 h (
  2. customuntil completion of the reaction
  3. customMost of the solvents were removed by distillation
  4. additionthe residue was dispersed in a mixture of water (30 mL) and methanol (30 mL)
  5. additionThe mixture was treated with charcoal
  6. filtrationfiltered
  7. filtrationThe resulting precipitate was collected by filtration
  8. washwashed with water
  9. customdried (yield: 0.29 g)

Quellen und Nachweise

ORD-Eintrag
ord-5223e56f476842e78541340a7fe3b0ae
Quelldatensatz
uspto-grants-1998_08
Patentnummer
US05792764

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