Ethanol → HCID 136238744, compound

HRID 2278525Notes

Reaction equation

HRID 2278525 reaction equation
[CH3:1][CH:2]1[O:7][CH2:6][CH2:5][NH:4][CH2:3]1.Cl.C(O[C:12](=[NH:19])[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])C.C([N:23]([CH2:27][CH3:28])C(C)C)(C)C.[CH2:29]([OH:31])C>>[CH2:17]([O:16][C:14](=[O:15])[CH2:13][C:12]1[NH:19][C:29](=[O:31])[CH:28]=[C:27]([N:4]2[CH2:5][CH2:6][O:7][CH:2]([CH3:1])[CH2:3]2)[N:23]=1)[CH3:18]

Participants

5

Reactant 4

HCID 702EthanolHCID 75345Ethyl 3-ethoxy-3-iminopropionate hydrochlorideHCID 81531DiisopropylethylamineHCID 4106152-Methylmorpholine

Product 1

HCID 136238744HCID 136238744, compound

Procedure

20 ml of ethanol, 1.5 g of 2-methylmorpholine, 8.7 g of ethyl 3-ethoxy-3-iminopropanoate hydrochloride and 7.75 ml of N,N-diisopropylethylamine are placed in a microwave tube. After one hour of microwave irradiation at a temperature of 130° C., the reaction medium is concentrated under reduced pressure. The residue obtained is purified on a silica column, eluent: dichloromethane/methanol: 97/03, so as to give 0.8 g of [4-(2-methylmorpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetic acid ethyl ester in the form of a beige solid, the characteristics of which are the following:

Workup

  1. customAfter one hour of microwave irradiation at a temperature of 130° C.
  2. concentrationthe reaction medium is concentrated under reduced pressure
  3. customThe residue obtained
  4. customis purified on a silica column, eluent

Sources & evidence

ORD record
ord-3f019680146c4f5b8233cec4c0bfea23
Source dataset
uspto-grants-2015_09
Patent number
US09133168B2

Reaction notes

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