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HRID 1496819作成日:2026年10月27日

Hydrochloric Acid → 945667-22-1

https://huagongshe.com/reaction/1496819

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SaxagliptinHCID 11243969—
溶媒DichloromethaneHCID 6344—
生成物945667-22-1HCID 5329747375%

反応条件

温度27.5 °C

反応手順

The compound of Boc protected (amino group protected by Di-tert-butyl dicarbonate group) saxagliptin (5.0 g gm) was dissolved in methylene chloride (40 ml); and the concentrated hydrochloric acid (4 ml) was added to the above solution. The reaction mixture was stirred for 4 hrs at 25-30° C. After the completion of the reaction, purified water (40 ml) was added to the reaction mixture at 25-30° C. and the pH was adjusted to 9-10 by the addition of potassium carbonate at the same temperature. Methylene chloride (20 ml) was added to the reaction mixture and stirred. The methylene chloride layer was separated and distilled under vacuum. The resulting residue was mixed with ethylacetate (25 ml) and treated with purified water. The contents were stirred, the resultant solid was filtered under vacuum and dried at 50-55° C. for 6 hrs. Yield: 75%.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09199933B2
出典データセットuspto-grants-2015_12
ORD IDord-b7fad8f2def04bb1bb7c303dfdf508ce
出典メモuspto-grants-2015_12