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

HRID 473848

Reaktionsgleichung

Reaktionsgleichung von HRID 473848
[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 4M 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-3d1c6b8d66da4b39b979a793961ed21b
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08637499B2

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