Hydrochloric Acid → Dibenzo[b,f][1,4]thiazepin-11-ylamine hydrochloride

HRID 1967183Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1967183
[ClH:1].[CH:2]1[C:7]2[C:8]([NH2:17])=[N:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[S:12][C:6]=2[CH:5]=[CH:4][CH:3]=1>CC(O)C.C(O)(C)C.COC(C)(C)C>[ClH:1].[CH:2]1[C:7]2[C:8]([NH2:17])=[N:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[S:12][C:6]=2[CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 374037Dibenzo(b,f)(1,4)thiazepin-11-amine

Produkt 1

HCID 44158775Dibenzo[b,f][1,4]thiazepin-11-ylamine hydrochlorideAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3776IsopropanolLösungsmittelHCID 86616950TBME isopropanolLösungsmittel

Versuchsvorschrift

A solution of gaseous HCl in i-PrOH (5.7 g, 31 wt-%) was added dropwise under stirring to a solution of dibenzo[b,f][1,4]thiazepin-11-ylamine (10.6 g) dissolved in a isopropanol/tert-butyl methyl ether (TBME) mixture (150 ml/120 ml). Stirring was continued for 1 h and the formed precipitate was filtered off, washed with tert-butyl methyl ether (TBME) and dried on air to obtain the desired compound as a colorless solid (11.2 g, 91%).

Aufarbeitung

  1. filtrationthe formed precipitate was filtered off
  2. washwashed with tert-butyl methyl ether (TBME)
  3. customdried on air

Quellen und Nachweise

ORD-Eintrag
ord-79876ac24f6346eb98e31d846d8fd968
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08420807B2

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