Sulfuric acid magnesium salt (1:1) → HCID 15136143, compound

HRID 1651044Notes

Reaction equation

HRID 1651044 reaction equation
[NH:1]1[CH2:6][CH2:5][S:4][CH2:3][CH2:2]1.S([O-])([O-])(=O)=O.[Mg+2].[CH2:13]([O:15][C:16]([C:18]1[C:23](=[O:24])[N:22]2[CH:25]=[CH:26][CH:27]=[C:28]([S:29][CH2:30]O)[C:21]2=[N:20][CH:19]=1)=[O:17])[CH3:14]>O1CCCC1>[CH2:13]([O:15][C:16]([C:18]1[C:23](=[O:24])[N:22]2[CH:25]=[CH:26][CH:27]=[C:28]([S:29][CH2:30][N:1]3[CH2:6][CH2:5][S:4][CH2:3][CH2:2]3)[C:21]2=[N:20][CH:19]=1)=[O:17])[CH3:14]

Participants

5

Reactant 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 67164ThiomorpholineHCID 56611467HCID 56611467, compound

Product 1

HCID 15136143HCID 15136143, compoundYield 54.9%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

To a mixture of 163 mg of thiomorpholine, 920 mg of magnesium sulfate and 5 ml of tetrahydrofuran is added dropwise a solution of 429 mg of 3-ethoxycarbonyl-9-(hydroxymethylthio)-4-oxo-4H-pyrido[1,2-a]pyrimidine (III) in 25 ml of tetrahydrofuran with stirring under ice-cooling. The reaction mixture is stirred for 1 hour as it is, filtered, and the filtrate is concentrated in vacuo. The residue is recrystallized from ethyl acetatehexane to give 307 mg (Yield: 54.9%) of 3-ethoxycarbonyl-9-(thiomorpholinomethylthio)-4-oxo-4H-pyrido[1,2-a]pyrimidine (I c-1).

Workup

  1. temperaturecooling
  2. stirringThe reaction mixture is stirred for 1 hour as it
  3. filtrationfiltered
  4. concentrationthe filtrate is concentrated in vacuo
  5. customThe residue is recrystallized from ethyl acetatehexane

Sources & evidence

ORD record
ord-9e720b4dc39445fe8edecf54952c01ad
Source dataset
uspto-grants-1990_05
Patent number
US04927829

Reaction notes

Loading…