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

HRID 1460478Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1460478
[ClH:1].[CH3:2][O:3][C:4]1[CH:32]=[CH:31][C:7]([CH2:8][CH2:9][N:10]2[CH2:14][CH2:13][CH2:12][C@H:11]2[CH2:15][N:16]2[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[CH2:20][S:19][C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]2=3)=[CH:6][CH:5]=1>CCOCC>[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[CH:6][C:7]([CH2:8][CH2:9][N:10]2[CH2:14][CH2:13][CH2:12][C@H:11]2[CH2:15][N:16]2[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[CH2:20][S:19][C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]2=3)=[CH:31][CH:32]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 9824029(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine

Produkt 1

HCID 67834802(S)-5,11-Dihydro-5-[1-(4-methoxyphenethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine hydrochlorideAusbeute 43 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

Excess saturated ethereal hydrogen chloride solution 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) (1.30 g) in ether (20 ml) and the mixture was stirred at room temperature for 16 hours. The resulting precipitate was collected, washed several times with ether, dried and recrystallised from ethyl acetate to give the title compound as colourless crystals, (602 mg, 43%), m.p. 189°-190° C., [α]58925 -30.7° (c=0.57 in ethanol).

Aufarbeitung

  1. customThe resulting precipitate was collected
  2. washwashed several times with ether
  3. customdried
  4. customrecrystallised from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-a5f26e2f2374407f8ce6101c199d214e
Quelldatensatz
uspto-grants-1991_12
Patentnummer
US05071844

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