Methanol → 10,11-Dihydrodibenzo(b,f)(1,4)thiazepine

HRID 962503

Reaktionsgleichung

Reaktionsgleichung von HRID 962503
O=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[NH:3]1.B.CSC.CO>O1CCCC1>[CH:9]1[C:8]2[CH2:2][NH:3][C:4]3[CH:16]=[CH:15][CH:14]=[CH:13][C:5]=3[S:6][C:7]=2[CH:12]=[CH:11][CH:10]=1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 374829DibenzothiazepinoneHCID 12423031(Dimethyl sulfide)trihydroboron

Produkt 1

HCID 1231048210,11-Dihydrodibenzo(b,f)(1,4)thiazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a mixture of 3.3 g of 10,11-dihydro-11-oxodibenz[b,f] [1,4]thiazepine in 25 ml of tetrahydrofuran is added 4.0 ml of 10 molar borane-dimethylsulfide in tetrahydrofuran. The mixture is stirred at room temperature for 18 hours, 50 ml of anhydrous methanol added and the solvent removed. An additional 30 ml of methanol is added and the solvent removed to give white crystals. A sample is purified by chromatography on silica gel with hexane-chloroform-ethyl acetate (2:1:1) as solvent to give white crystals, m.p. 145°-148° C.

Aufarbeitung

  1. customthe solvent removed
  2. additionAn additional 30 ml of methanol is added
  3. customthe solvent removed
  4. customto give white crystals
  5. customA sample is purified by chromatography on silica gel with hexane-chloroform-ethyl acetate (2:1:1) as solvent
  6. customto give white crystals, m.p. 145°-148° C.

Quellen und Nachweise

ORD-Eintrag
ord-0d2ca8e5867c4fff846e7e5a15043659
Quelldatensatz
uspto-grants-1998_06
Patentnummer
US05760031

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