Morpholine → (4-Methoxy-6-morpholin-4-ylpyrimidin-2-yl)acetic acid ethyl ester

HRID 2278582Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2278582
[CH2:1]([O:3][C:4](=[O:15])[CH2:5][C:6]1[N:11]=[C:10](Cl)[CH:9]=[C:8]([O:13][CH3:14])[N:7]=1)[CH3:2].[NH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1>>[CH2:1]([O:3][C:4](=[O:15])[CH2:5][C:6]1[N:7]=[C:8]([O:13][CH3:14])[CH:9]=[C:10]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)[N:11]=1)[CH3:2]

Komponenten

3

Edukt 2

HCID 8083MorpholineHCID 86699270Ethyl 2-(4-chloro-6-methoxypyrimidin-2-yl)acetate

Produkt 1

HCID 86699276(4-Methoxy-6-morpholin-4-ylpyrimidin-2-yl)acetic acid ethyl ester

Versuchsvorschrift

1.5 g of (4-chloro-6-methoxypyrimidin-2-yl)acetic acid ethyl ester and 20 ml of morpholine are mixed together in a microwave tube. After microwave irradiation for 1 h at 90° C., the reaction mixture is concentrated under reduced pressure and then diluted with 300 ml of ethyl acetate and 300 ml of water. After settling out, the organic phase is dried over magnesium sulfate, filtered, and then concentrated under reduced pressure. 1.9 g of (4-methoxy-6-morpholin-4-ylpyrimidin-2-yl)acetic acid ethyl ester are thus obtained in the form of a viscous oil which crystallizes and which is used as it is in the next step.

Aufarbeitung

  1. customAfter microwave irradiation for 1 h at 90° C.
  2. concentrationthe reaction mixture is concentrated under reduced pressure
  3. additiondiluted with 300 ml of ethyl acetate and 300 ml of water
  4. dry with materialthe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6d774c6aa84c41fe889eaa301b69859f
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09133168B2

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