(3-甲基硫杂环丁烷-3-基)甲醇

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N,N-Dimethylformamide dineopentyl acetal (2.72 ml) was added to a stirred suspension of 5-chloropyrimidin-2-one (789 mg) and 3-hydroxymethyl-3-methylthietane (1.000 g) in dry N,N-dimethylformamide (15 ml) under nitrogen and the mixture was then heated at 100° C. After 42.5 h the reaction mixture was evaporated and the resulting black residue was dissolved in ethyl acetate (300 ml), washed with water (3×70 ml), dried (MgSO4) and evaporated to a dark brown gum. Trituration of the gum with diethyl ether gave a pale brown solid which was crystallised from ethyl acetate to give cream crystals of the title pyrimidinone (110 mg), m.p. 200°-202° C., νmax (nujol) 1663, 1510 cm-1 (C=O), 1612, 1582 cm-1 (C=C, C=N). After 42.5 h the reaction mixture was evaporated the resulting black residue was dissolved in ethyl acetate (300 ml) washed with water (3×70 ml) dried (MgSO4) evaporated to a dark brown gum Trituration of the gum with diethyl ether gave a pale brown solid which was crystallised from ethyl acetate

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N,N-Dimethylformamide dineopentyl acetal (2.72 ml) was added to a stirred suspension of 5-chloropyrimidin-2-one (789 mg) and 3-hydroxymethyl-3-methylthietane (1.000 g) in dry N,N-dimethylformamide (15 ml) under nitrogen and the mixture was then heated at 100° C. After 42.5 h the reaction mixture was evaporated and the resulting black residue was dissolved in ethyl acetate (300 ml), washed with water (3×70 ml), dried (MgSO4) and evaporated to a dark brown gum. Trituration of the gum with diethyl ether gave a pale brown solid which was crystallised from ethyl acetate to give cream crystals of the title pyrimidinone (110 mg), m.p. 200°-202° C., νmax (nujol) 1663, 1510 cm-1 (C=O), 1612, 1582 cm-1 (C=C, C=N). After 42.5 h the reaction mixture was evaporated the resulting black residue was dissolved in ethyl acetate (300 ml) washed with water (3×70 ml) dried (MgSO4) evaporated to a dark brown gum Trituration of the gum with diethyl ether gave a pale brown solid which was crystallised from ethyl acetate

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N,N-Dimethylformamide dineopentyl acetal (2.72 ml) was added to a stirred suspension of 5-chloropyrimidin-2-one (789 mg) and 3-hydroxymethyl-3-methylthietane (1.000 g) in dry N,N-dimethylformamide (15 ml) under nitrogen and the mixture was then heated at 100° C. After 42.5 h the reaction mixture was evaporated and the resulting black residue was dissolved in ethyl acetate (300 ml), washed with water (3×70 ml), dried (MgSO4) and evaporated to a dark brown gum. Trituration of the gum with diethyl ether gave a pale brown solid which was crystallised from ethyl acetate to give cream crystals of the title pyrimidinone (110 mg), m.p. 200°-202° C., νmax (nujol) 1663, 1510 cm-1 (C=O), 1612, 1582 cm-1 (C=C, C=N). After 42.5 h the reaction mixture was evaporated the resulting black residue was dissolved in ethyl acetate (300 ml) washed with water (3×70 ml) dried (MgSO4) evaporated to a dark brown gum Trituration of the gum with diethyl ether gave a pale brown solid which was crystallised from ethyl acetate