Hydroxyamine hydrochloride → HCID 178452412, Verbindung

HRID 1514228Notizen

Reaktionsgleichung

[C:1]([C:3]1[C:13]2[O:12][CH2:11][CH2:10][N:9]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1)#[N:2].Cl.[NH2:22][OH:23].C(=O)(O)[O-].[Na+]>C(O)C>[OH:23][NH:22][C:1](=[NH:2])[C:3]1[C:13]2[O:12][CH2:11][CH2:10][N:9]([C:14]([O:16][C:17]([CH3:19])([CH3:18])[CH3:20])=[O:15])[CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1

Komponenten

Reaktionsbedingungen

Temperatur: 60 °C

Versuchsvorschrift

A suspension of 1,1-dimethylethyl 9-cyano-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (Preparation 64) (5.1 g, 18.59 mmol), hydroxylamine hydrochloride (2.58 g, 37.2 mmol) and sodium bicarbonate (7.81 g, 93 mmol) in ethanol (50 ml) was heated at 60° C. overnight. A further portion of hydroxylamine hydrochloride (1 g) was added and the reaction was heated at 60° C. overnight. The solid was filtered from the reaction mixture and the filtrate evaporated. The residue from the evaporation was dissolved in EtOAc, washed with water, dried over magnesium sulphate and evaporated. Trituration with ether to gave the title compound (3.94 g) as a white solid. MS (ES): C15H21N3O4 requires 307; found 308 [M+H]+.

Aufarbeitung

temperaturethe reaction was heated at 60° C. overnight
filtrationThe solid was filtered from the reaction mixture
customthe filtrate evaporated
customThe residue from the evaporation
dissolutionwas dissolved in EtOAc
washwashed with water
dry with materialdried over magnesium sulphate
customevaporated

Quellen und Nachweise

ORD-Eintrag: ord-c0d46a05387248558d159f24a420a158
Quelldatensatz: uspto-grants-2012_07
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08222245B2

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