Hydrogen chloride-ethyl acetate → 9-[(1Z)-propa-1-ene-1-yl]-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride

HRID 886932Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 886932
[CH:1](/[C:4]1[C:14]2[O:13][CH2:12][CH2:11][N:10](C(OC(C)(C)C)=O)[CH2:9][C:8]=2[CH:7]=[CH:6][CH:5]=1)=[CH:2]/[CH3:3].C(OCC)(=O)C.[ClH:28]>C(OCC)(=O)C>[ClH:28].[CH:1](/[C:4]1[C:14]2[O:13][CH2:12][CH2:11][NH:10][CH2:9][C:8]=2[CH:7]=[CH:6][CH:5]=1)=[CH:2]/[CH3:3]

Komponenten

4

Edukt 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 68578267tert-butyl 9-[(1Z)-propa-1-ene-1-yl]-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

Produkt 1

HCID 685794579-[(1Z)-propa-1-ene-1-yl]-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochlorideAusbeute 90,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A mixture of tert-butyl 9-[(1Z)-propa-1-ene-1-yl]-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (170 mg, 0.587 mmol), ethyl acetate (1 ml) and 4N hydrogen chloride-ethyl acetate solution (2 ml) was stirred at room temperature for 1 hr, and the solvent was evaporated under reduced pressure. The residue was recrystallized from a mixed solvent of methanol and ether to give the desired product (120 mg, 90.9%) as a solid.

Aufarbeitung

  1. customthe solvent was evaporated under reduced pressure
  2. customThe residue was recrystallized from a mixed solvent of methanol and ether

Quellen und Nachweise

ORD-Eintrag
ord-252681645bf1487c80768ba5c61285ad
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08247403B2

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