m-Chloroperbenzoic acid → HCID 12953049, compound

HRID 904557Notes

Reaction equation

HRID 904557 reaction equation
[O:1]=[C:2]1[N:7]2[CH:8]=[C:9]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:10]=[CH:11][C:6]2=[N:5][C:4]2[CH2:17][S:18][CH2:19][C:3]1=2.ClC1C=CC=C(C(OO)=O)C=1>C(Cl)(Cl)Cl>[O:1]=[C:2]1[N:7]2[CH:8]=[C:9]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:10]=[CH:11][C:6]2=[N:5][C:4]2=[CH:17][S:18][CH:19]=[C:3]12

Participants

4

Reactant 2

HCID 70297m-Chloroperbenzoic acidHCID 12953041HCID 12953041, compound

Product 1

HCID 12953049HCID 12953049, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

A mixture of ethyl 3,10-dihydro-10-oxo-1H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carboxylate (2.0 g., 0.0072 mol) and m-chloroperbenzoic acid (1.47 g., 0.0072 mol) in chloroform (75 ml) is stirred at room temperature overnight. The solvent is evaporated at reduced pressure to give a syrup, which crystallizes from ethanol. Recrystallization from ethanol, silica gel chromatography and a further recrystallization from ethanol gives the product as yellow crystals (mp 175° C.).

Workup

  1. customThe solvent is evaporated at reduced pressure
  2. customto give a syrup, which
  3. customcrystallizes from ethanol
  4. customRecrystallization from ethanol, silica gel chromatography
  5. customa further recrystallization from ethanol

Sources & evidence

ORD record
ord-e08c140532bc4395b5df6e35b574837b
Source dataset
uspto-grants-1980_10
Patent number
US04230707

Reaction notes

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