Methanesulfonic Acid → (S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine methanesulphonate

HRID 1460476Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1460476
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:36]=[CH:35][C:11]([CH2:12][CH2:13][N:14]2[CH2:18][CH2:17][CH2:16][C@H:15]2[CH2:19][N:20]2[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[CH2:24][S:23][C:22]3[CH:31]=[CH:32][CH:33]=[CH:34][C:21]2=3)=[CH:10][CH:9]=1>ClCCl>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:9]=[CH:10][C:11]([CH2:12][CH2:13][N:14]2[CH2:18][CH2:17][CH2:16][C@H:15]2[CH2:19][N:20]2[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[CH2:24][S:23][C:22]3[CH:31]=[CH:32][CH:33]=[CH:34][C:21]2=3)=[CH:35][CH:36]=1

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 9824029(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine

Produkt 1

HCID 88452751(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine methanesulphonateAusbeute 70,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Methanesulphonic acid (39 mg) was added to a solution of (S)-5,11-dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine (see Examples 1 and 6) (175 mg) in dichloromethane (5 ml) and the mixture was stirred at room temperature for 16 hours and evaporated under reduced pressure. The residue was crystallised from ethyl acetate/diisopropyl ether to give the title compound as colourless crystals, (150 mg, 31%), m.p. 118°-122° C., [α]58925 -36.9° (c=0.59 in ethanol).

Aufarbeitung

  1. customevaporated under reduced pressure
  2. customThe residue was crystallised from ethyl acetate/diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-71a82233e1a1419aa062770e9915adcd
Quelldatensatz
uspto-grants-1991_12
Patentnummer
US05071844

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