Water → 1,4-Dioxa-8-aza-spiro[4.5]decane-8-carbonitrile

HRID 1409685Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1409685
[O:1]1[C:5]2([CH2:10][CH2:9][NH:8][CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[CH2:11]([N:13](C(C)C)C(C)C)C.O>ClCCl.O1CCCC1>[O:1]1[C:5]2([CH2:10][CH2:9][N:8]([C:11]#[N:13])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1

Komponenten

6

Edukt 3

HCID 962WaterHCID 674351,4-Dioxa-8-azaspiro(4.5)decaneHCID 81531Diisopropylethylamine

Produkt 1

HCID 866782101,4-Dioxa-8-aza-spiro[4.5]decane-8-carbonitrile

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Bromonitrile (11.12 g) is added to a mixture of 1,4-dioxa-8-aza-spiro[4.5]decane (10.00 g) and ethyldiisopropylamine (59.92 mL) in dichloromethane (125 mL) and tetrahydrofuran (125 mL). The reaction mixture is stirred over night at room temperature. Water is added and the organic phase is separated, dried over Na2SO4 and concentrated in vacuo to give the title compound. TLC: rf=0.80 (aluminum oxide, ethyl acetate/petrol ether 3:1); Mass spectrum (ESI+): m/z=169 [M+H]+.

Aufarbeitung

  1. customthe organic phase is separated
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d9c907ba963c4d56987eaca4366f4207
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08921398B2

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