苯氨基甲酸甲酯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: To a stirring solution of the N-oxide of 3-chloro-2-pyridinesulfonamide (85 mg, 0.4 mmol) and the phenyl carbamate of 4,6-dimethoxy-2-aminopyrimidine (114 mg, 0.40 mmol) in acetonitrile was added DBU (62 mg, 0.40 mmol). Addition of H2O followed by 5% HCl caused a precipitate to form which was collected, m.p. 144°-147° C. NMR (200 MHz, d6 -DMSO) δ 3.91 (s, 6H), 5.998 (s, 1H), 7.7 (m, 2H), 8.4 (d, 1H), 10.8 (br s, 1H) and 13.1 (br s, 1H); IR (nujol) 1710 (s) cm-1 ; mass spectrum m/e 390 (M+, calc. for C12H12ClN5O6S 389+1). to form which was collected

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

实验步骤: A mixture of 2.0 g (8.2 mmol) of the phenyl carbamate from Example 4a, 2 g (15 mmol) of K2CO3 and 1.3 g (10 mmol) of dimethyl sulfate in 20 ml of acetone is stirred for 3 hours at room temperature. The reaction mixture is then filtered and evaporated down, and the residue is purified by column chromatography with mixtures of cyclohexane and ethyl acetate. There is obtained 1.5 g (5.8 mmol =71%) of the title compound as a colorless oil, which slowly crystallizes (mp=60° C.). The reaction mixture is then filtered evaporated down the residue is purified by column chromatography with mixtures of cyclohexane and ethyl acetate

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

实验步骤: 3-[5-(N-methylsulfamoyl)-1,3,4-thiadiazol-2-yl]-1,1-dimethylurea, from 4 g. of the carbamic acid, phenyl ester, above, and 3 g. of diethylamine hydrochloride. The product had a melting point of about 152°-153° C. and weighed 1.5 g.

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

实验步骤: 3-[5-(N-methylsulfamoyl)-1,3,4-thiadiazol-2-yl]-1,1-dimethylurea, from 4 g. of the carbamic acid, phenyl ester, above, and 3 g. of diethylamine hydrochloride. The product had a melting point of about 152°-153° C. and weighed 1.5 g.

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

实验步骤: A mixture of 2.0 g (8.2 mmol) of the phenyl carbamate from Example 4a, 2 g (15 mmol) of K2CO3 and 1.3 g (10 mmol) of dimethyl sulfate in 20 ml of acetone is stirred for 3 hours at room temperature. The reaction mixture is then filtered and evaporated down, and the residue is purified by column chromatography with mixtures of cyclohexane and ethyl acetate. There is obtained 1.5 g (5.8 mmol{circumflex over (=)}71%) of the title compound as a colorless oil, which slowly crystallizes (mp=60° C.). The reaction mixture is then filtered evaporated down the residue is purified by column chromatography with mixtures of cyclohexane and ethyl acetate