2-chloroethylsulfonylmethylbenzene

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Amino-5-chloro-2-methoxy-N-(piperidin-4-ylmethyl)benzamide dihydrochloride (1.50 g) as a starting compound, 2-benzylsulfonylethyl chloride (1.21 g) and potassium carbonate (1.54 g) were reacted and treated in the same manner as in Example 199 to give 1.72 g of 4-amino-5-chloro-2-methoxy-N-((1-(2-benzylsulfonylethyl)piperidin-4-yl)methyl)-benzamide, treated in the same manner as in Example 199

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 51.49 g (0.236 mole) of benzyl 2-chloroethyl sulfone and 600 ml of isopropylamine was stirred at room temperature for 72 hr. The solvent was removed in vacuo, and the residue was partitioned between ether and dilute sodium hydroxide. The ether solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, and excess ethereal hydrogen chloride was added. Ether was added, and a white solid precipitated to give 43.11 g (65.8%) of a white crystalline solid, m.p. 180.5°-181.5° C. The solvent was removed in vacuo the residue was partitioned between ether and dilute sodium hydroxide The ether solution was dried over magnesium sulfate the solvent was removed in vacuo to give an oil a white solid precipitated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 51.49 g (0.236 mole) of benzyl 2-chloroethyl sulfone and 600 ml of isopropylamine was stirred at room temperature for 72 hr. The solvent was removed in vacuo, and the residue was partitioned between ether and dilute sodium hydroxide. The ether solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, and excess ethereal hydrogen chloride was added. Ether was added, and a white solid precipitated to give 43.11 g (65.8%) of a white crystalline solid, m.p. 180.5°-181.5° C. The solvent was removed in vacuo the residue was partitioned between ether and dilute sodium hydroxide The ether solution was dried over magnesium sulfate the solvent was removed in vacuo to give an oil a white solid precipitated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Amino-5-chloro-2-methoxy-N-(piperidin-4-ylmethyl)benzamide dihydrochloride (1.50 g) as a starting compound, 2-benzylsulfonylethyl chloride (1.21 g) and potassium carbonate (1.54 g) were reacted and treated in the same manner as in Example 199 to give 1.72 g of 4-amino-5-chloro-2-methoxy-N-((1-(2-benzylsulfonylethyl)piperidin-4-yl)methyl)-benzamide, treated in the same manner as in Example 199

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Amino-5-chloro-2-methoxy-N-(piperidin-4-ylmethyl)benzamide dihydrochloride (1.50 g) as a starting compound, 2-benzylsulfonylethyl chloride (1.21 g) and potassium carbonate (1.54 g) were reacted and treated in the same manner as in Example 199 to give 1.72 g of 4-amino-5-chloro-2-methoxy-N-((1-(2-benzylsulfonylethyl)piperidin-4-yl)methyl)-benzamide, treated in the same manner as in Example 199

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 51.49 g (0.236 mole) of benzyl 2-chloroethyl sulfone and 600 ml of isopropylamine was stirred at room temperature for 72 hr. The solvent was removed in vacuo, and the residue was partitioned between ether and dilute sodium hydroxide. The ether solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, and excess ethereal hydrogen chloride was added. Ether was added, and a white solid precipitated to give 43.11 g (65.8%) of a white crystalline solid, m.p. 180.5°-181.5° C. The solvent was removed in vacuo the residue was partitioned between ether and dilute sodium hydroxide The ether solution was dried over magnesium sulfate the solvent was removed in vacuo to give an oil a white solid precipitated

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 51.49 g (0.236 mole) of benzyl 2-chloroethyl sulfone and 600 ml of isopropylamine was stirred at room temperature for 72 hr. The solvent was removed in vacuo, and the residue was partitioned between ether and dilute sodium hydroxide. The ether solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, and excess ethereal hydrogen chloride was added. Ether was added, and a white solid precipitated to give 43.11 g (65.8%) of a white crystalline solid, m.p. 180.5°-181.5° C. The solvent was removed in vacuo the residue was partitioned between ether and dilute sodium hydroxide The ether solution was dried over magnesium sulfate the solvent was removed in vacuo to give an oil a white solid precipitated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 51.49 g (0.236 mole) of benzyl 2-chloroethyl sulfone and 600 ml of isopropylamine was stirred at room temperature for 72 hr. The solvent was removed in vacuo, and the residue was partitioned between ether and dilute sodium hydroxide. The ether solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, and excess ethereal hydrogen chloride was added. Ether was added, and a white solid precipitated to give 43.11 g (65.8%) of a white crystalline solid, m.p. 180.5°-181.5° C. The solvent was removed in vacuo the residue was partitioned between ether and dilute sodium hydroxide The ether solution was dried over magnesium sulfate the solvent was removed in vacuo to give an oil a white solid precipitated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-Amino-5-chloro-2-methoxy-N-(piperidin-4-ylmethyl)benzamide dihydrochloride (1.50 g) as a starting compound, 2-benzylsulfonylethyl chloride (1.21 g) and potassium carbonate (1.54 g) were reacted and treated in the same manner as in Example 199 to give 1.72 g of 4-amino-5-chloro-2-methoxy-N-((1-(2-benzylsulfonylethyl)piperidin-4-yl)methyl)-benzamide, treated in the same manner as in Example 199

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 51.49 g (0.236 mole) of benzyl 2-chloroethyl sulfone and 600 ml of isopropylamine was stirred at room temperature for 72 hr. The solvent was removed in vacuo, and the residue was partitioned between ether and dilute sodium hydroxide. The ether solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in methanol, and excess ethereal hydrogen chloride was added. Ether was added, and a white solid precipitated to give 43.11 g (65.8%) of a white crystalline solid, m.p. 180.5°-181.5° C. The solvent was removed in vacuo the residue was partitioned between ether and dilute sodium hydroxide The ether solution was dried over magnesium sulfate the solvent was removed in vacuo to give an oil a white solid precipitated