2,6-二乙基异硫氰酸苯酯

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

实验步骤: A solution of 1,3-diethyl-2-isothiocyanatobenzene (0.5 mmol) in 1:1 DMF/THF (2 mL) was reacted with 3,4-diamino-N-(1H-indazol-6-yl)-benzamide (0.5 mmol; see Example 25) according to general procedure B to yield 2-(2,6-diethylphenylamino)-3H-benzimidazole-5-carboxylic acid (1H-indazol-6-yl)-amide. MS: m/z 425 (M+H)+.

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

实验步骤: A solution of 1,3-diethyl-2-isothiocyanatobenzene (0.5 mmol) in 1:1 DMF/THF (2 mL) was reacted with 3,4-diamino-N-(1H-indazol-6-yl)-benzamide (0.5 mmol; see Example 25) according to general procedure B to yield 2-(2,6-diethylphenylamino)-3H-benzimidazole-5-carboxylic acid (1H-indazol-6-yl)-amide. MS: m/z 425 (M+H)+.

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

实验步骤: Reaction of 2,6-diethyl-phenyl isothiocyanate with isopropylamine in accordance with the process described above gives N-(2,6-diethyl-phenyl)-N'-isopropyl-thiourea of melting point: 108° to 110°.

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

实验步骤: 2,6-Diethyl-phenyl isothiocyanate can be prepared as follows: 100 g of 2,6-diethylaniline in 200 ml of methylene chloride are added dropwise at 0°-5°, whilst stirring, to a mixture of 500 ml of methylene chloride, 300 ml of water, 120 g of calcium carbonate and 92 g of thiophosgene. The mixture is then heated to the reflux temperature until the evolution of CO2 has ended. The cooled batch is filtered and the methylene chloride layer is separated off, dried with calcium chloride and fractionated. The cooled batch is filtered the methylene chloride layer is separated off dried with calcium chloride

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

实验步骤: To a stirred suspension of 7.3 g (30.0 mmol) of methylguanidine sulfate in THF (100 ml) was added 4.8 g (60.0 mmol) of 50% W/W aqueous NaOH. The mixture was stirred for one hour after which 5.0 g of anhydrous Na2SO4 was added and the mixture stirred for an additional hour. To the mixture was added dropwise over one hour a solution of 5.7 g (30.0 mmol) of 2,6-diethylphenylisothiocyanate in THF (40 ml) and the mixture was stirred for two hours at ambient temperature. The THF was removed under vacuum and the residue partitioned between H2O and CHCl3. The layers were separated and the aqueous layer extracted with CHCl3 (1×100 ml). The extracts were dried (MgSO4) and concentrated to give a yellow oil which was dissolved in MeOH and acidified with HCl/MeOH. The MeOH was removed under vacuum to give a viscous yellow oil which slowly crystallized on standing. Crystallization from MeOH/CH3C≡N gave 8.5 g (94 %) of the desired salt. was added the mixture was stirred for two hours at ambient temperature The THF was removed under vacuum the residue partitioned between H2O and CHCl3 The layers were separated the aqueous layer extracted with CHCl3 (1×100 ml) The extracts were dried (MgSO4) concentrated to give a yellow oil which The MeOH was removed under vacuum to give a viscous yellow oil which slowly crystallized Crystallization from MeOH/CH3C≡N

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

实验步骤: A solution of 1,3-diethyl-2-isothiocyanatobenzene (0.5 mmol) in 1:1 DMF/THF (2 mL) was reacted with 3,4-diamino-N-(1H-indazol-6-yl)-benzamide (0.5 mmol; see Example 25) according to general procedure B to yield 2-(2,6-diethylphenylamino)-3H-benzimidazole-5-carboxylic acid (1H-indazol-6-yl)-amide. MS: m/z 425 (M+H)+.

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

实验步骤: A solution of 1,3-diethyl-2-isothiocyanatobenzene (0.5 mmol) in 1:1 DMF/THF (2 mL) was reacted with 3,4-diamino-N-(1H-indazol-6-yl)-benzamide (0.5 mmol; see Example 25) according to general procedure B to yield 2-(2,6-diethylphenylamino)-3H-benzimidazole-5-carboxylic acid (1H-indazol-6-yl)-amide. MS: m/z 425 (M+H)+.