Hydrochloric Acid → 7-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride

HRID 241087

Reaktionsgleichung

Reaktionsgleichung von HRID 241087
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][CH2:9][N:8](C(OC(C)(C)C)=O)[CH2:7][C:6]=2[CH:19]=1.C(O)C.[ClH:23].O1CCOCC1>C(OCC)C>[ClH:23].[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][CH2:9][NH:8][CH2:7][C:6]=2[CH:19]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 312751,4-DioxaneHCID 25220760tert-Butyl 7-bromo-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

Produkt 1

HCID 668201377-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochlorideAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

1,1-dimethylethyl 7-bromo-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (10 g, 30.5 mmol) was taken into hot ethanol (10 mL) followed by addition of 4 M hydrogen chloride in dioxane solution (2.1 eq, 16 mL) and the resulting solution was allowed to slowly cool to ambient temperature over one hour. An excess of ethyl ether was then added and the resulting slurry was filtered. The filter cake was washed with ethyl ether and dried to give 7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride (7.9 g, 98% yield) as a colorless crystalline solid. MS (EI) for C9H10NOBr: 229 (MH+).

Aufarbeitung

  1. filtrationthe resulting slurry was filtered
  2. washThe filter cake was washed with ethyl ether
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-236090125a054c49b7aaa8c573f5deca
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08648066B2

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