Potassium Carbonate → HCID 15729187、化合物

温度

90 °C

A mixture of 2-amino-5-bromothiazole hydrochloride (2.2 g), 4-amino-2-mercaptopyrimidine (2.2 g) and potassium carbonate (6.5 g) in N,N-dimethylformamide (100 ml) was heated at 90° C. for 2.5 hours with stirring. The reaction mixture was concentrated under reduced pressure and water was added to this residue. The solution was extracted with a mixture of tetrahydrofuran and ethyl acetate (1:1), washed with aqueous saturated sodium chloride and dried over magnesium sulfate. The solvent was concentrated under reduced pressure to give solid. The solid was subjected to column chromatography on silica gel (silica gel 60, 70-230 mesh; Merck: 250 g) and eluted with a mixture of chloroform and methanol (10:1). The fractions containing the objective compound were combined and concentrated under reduced pressure to give solid. The solid was triturated with ethanol to give 2-amino-5-(4-aminopyrimidin-2-ylthio)thiazole (1.25 g, yield: 55.6%). mp: 185°-187° C. (dec.)

1. concentrationThe reaction mixture was concentrated under reduced pressure and water
2. additionwas added to this residue
3. extractionThe solution was extracted with a mixture of tetrahydrofuran and ethyl acetate (1:1)
4. washwashed with aqueous saturated sodium chloride
5. dry with materialdried over magnesium sulfate
6. concentrationThe solvent was concentrated under reduced pressure
7. customto give solid
8. washeluted with a mixture of chloroform and methanol (10:1)
9. additionThe fractions containing the objective compound
10. concentrationconcentrated under reduced pressure
11. customto give solid
12. customThe solid was triturated with ethanol

ORDレコード

ord-b7c39f16b39c40458976f68ae234dece

出典データセット

uspto-grants-1993_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05256675