HCID 53944659, Verbindung → 2-(Morpholin-4-yl)pyrimidine-5-carboxylic acid

HRID 1907707Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1907707
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:12]=[CH:11][C:10]([C:13]([O:15]CC)=[O:14])=[CH:9][N:8]=2)[CH2:3][CH2:2]1>Cl.O>[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:8]=[CH:9][C:10]([C:13]([OH:15])=[O:14])=[CH:11][N:12]=2)[CH2:3][CH2:2]1

Komponenten

4

Edukt 1

HCID 53944659HCID 53944659, Verbindung

Produkt 1

HCID 31609792-(Morpholin-4-yl)pyrimidine-5-carboxylic acidAusbeute 107,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

A solution of ester 122 (0.205 g, 0.86 mmol) in 2N HCl in H2O (10 mL) was stirred at 110° C. in a pressure vessel for 6 h, cooled to −78° C. and lyophilized for 2 days. The resulting amorphous solid was further dried using a mixture of dry acetonitrile (10 mL) and dry benzene (10 mL) followed by concentration (this was repeated 3 times) to give compound 123 (0.193 g, 92% yield). LRMS: 209.1 (calc) 210.0 (obs).

Aufarbeitung

  1. customThe resulting amorphous solid was further dried
  2. additiona mixture of dry acetonitrile (10 mL) and dry benzene (10 mL)
  3. concentrationfollowed by concentration (

Quellen und Nachweise

ORD-Eintrag
ord-6e224ce6bbbc4b14ae7d568535675e76
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08598168B2

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