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HRID 55055作成日:2026年10月24日

Hydrochloric Acid → 6-Carboxy-3-[1-(6,7-dimethoxy-4-quinazolinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-1-methyl-2,4-dioxo-quinazoline

https://huagongshe.com/ja/reaction/55055

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物Sodium HydroxideHCID 14798—
反応物BromineHCID 24408—
反応物Hypobromous acidHCID 83547—
反応物6-Acetyl-3-[1-(6,7-dimethoxy-4-quinazolinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-1-methyl-2,4-dioxo-quinazolineHCID 22923373—
溶媒ChloroformHCID 6212—
溶媒1,4-DioxaneHCID 31275—
生成物6-Carboxy-3-[1-(6,7-dimethoxy-4-quinazolinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-1-methyl-2,4-dioxo-quinazolineHCID 2292338821.3%

反応手順

In a solvent mixture of 30 ml of 1,4-dioxane and 5 ml of chloroform was suspended 245.0 mg (0.50 mmol) of Compound 63 obtained in Example 50. The suspension was added to a solution of hypobromous acid (3 mmol) which was prepared by adding 0.15 ml of bromine to a solvent mixture of 3 ml of a 2N aqueous solution of sodium hydroxide and 1 ml of 1,4-dioxane under ice cooling. The mixture was stirred at room temperature for one day, and then neutralized by addition of 4N hydrochloric acid, followed by extraction with chloroform. The organic layer was washed and dried, and the solvent was distilled off under reduced pressure. To the residue was added ether, and the precipitated crystals were collected by filtration and dried to give 52.4 mg (yield: 21%) of Compound 62 as white crystals.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05624926
出典データセットuspto-grants-1997_04
ORD IDord-5671186726a84749a382b44035b9f6a9
出典メモuspto-grants-1997_04