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Hydrochloric Acid → N,N-dimethyl-1-[6-(1-naphthylsulfonyl)-2,3-dihydro[1,4]oxazino[2,3,4-hi]indazol-2-yl]methanamine Hydrochloride

HRID 33111
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 33111
[Cl:1][CH2:2][CH:3]1[CH2:13][N:12]2[C:14]3[C:9]([C:10]([S:15]([C:18]4[C:27]5[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=5)[CH:21]=[CH:20][CH:19]=4)(=[O:17])=[O:16])=[N:11]2)=[CH:8][CH:7]=[CH:6][C:5]=3[O:4]1.[CH3:28][NH:29][CH3:30].Cl.CCOCC>CS(C)=O.O>[ClH:1].[CH3:28][N:29]([CH3:30])[CH2:2][CH:3]1[O:4][C:5]2=[C:14]3[C:9](=[CH:8][CH:7]=[CH:6]2)[C:10]([S:15]([C:18]2[C:27]4[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=4)[CH:21]=[CH:20][CH:19]=2)(=[O:17])=[O:16])=[N:11][N:12]3[CH2:13]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 3283Diethyl EtherHCID 251690347-Chloromethyl-2(naphthalene-1-sulfonyl)-7,8-dihydro-6-oxa-1,8a-diaza-acenaphthylene

Produkt 1

HCID 25169296N,N-dimethyl-1-[6-(1-naphthylsulfonyl)-2,3-dihydro[1,4]oxazino[2,3,4-hi]indazol-2-yl]methanamine Hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 7-chloromethyl-2-(naphthalene-1-sulfonyl)-7,8-dihydro-6-oxa-1,8a-diaza-acenaphthylene (0.075 g, 0.18 mmoles) and dimethylamine (0.56 ml, 1M solution in THF, 0.56 mmoles) in DMSO was stirred under nitrogen at 100° C. for 4 hours, cooled to room temperature, diluted with water and extracted with EtOAc. The extracts were combined, washed sequentially with water and brine, dried over Na2SO4 and concentrated under vacuum. The resultant residue was purified by flash chromatography using as eluent 5% CH3OH/EtOAc. The purified compound was dissolved in methanol, treated with 1M HCl in ether (0.2 ml, 0.2 mmoles) and evaporated to dryness to afford the title compound, MS: (ES) m/z 407.

Aufarbeitung

  1. temperaturecooled to room temperature
  2. extractionextracted with EtOAc
  3. washwashed sequentially with water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under vacuum
  6. customThe resultant residue was purified by flash chromatography
  7. dissolutionThe purified compound was dissolved in methanol
  8. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-54107132d07d48338dc750a18208c17c
Quelldatensatz
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07429582B2

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