2-Aminopropanol → HCID 178460116, Verbindung

HRID 481970

Reaktionsgleichung

Reaktionsgleichung von HRID 481970
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.[NH2:16][CH:17]([CH3:20])[CH2:18][OH:19]>C(OCC)C>[OH:19][CH2:18][CH:17]([NH:16][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)[CH3:20]

Komponenten

4

Edukt 2

HCID 51262-AminopropanolHCID 190647513-Methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate

Produkt 1

HCID 178460116HCID 178460116, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A suspension of 3-methylsulfanyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-dioxide monohydrate and 2-amino-1-propanol (0.75 mL) was refluxed for 90 min (until completion of the reaction; t.l.c.). After cooling, the addition of diethylether (20 mL) gave rise to the separation of an oily residue. After decantation of the etheral solution, the residue was solubilized in methanol (1 mL) and then supplemented with diethylether (15 mL). An oily residue separated again. After decantation of the supernatent, the oily residue was solubilized in acetone (6 mL). A fine precipitate readily appeared. After 3 h at +4° C., the resulting precipitate was collected by filtration, washed with acetone and dried (yield: 0.33 g); m.p. 213°-216° C. (Compound 19).

Aufarbeitung

  1. temperaturewas refluxed for 90 min (
  2. customuntil completion of the reaction
  3. temperatureAfter cooling
  4. customgave rise
  5. customto the separation of an oily residue
  6. customAn oily residue separated again
  7. filtrationthe resulting precipitate was collected by filtration
  8. washwashed with acetone
  9. customdried (yield: 0.33 g)

Quellen und Nachweise

ORD-Eintrag
ord-c0c6d6652c6e44438236c643e2c99a69
Quelldatensatz
uspto-grants-1998_08
Patentnummer
US05792764

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