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HRID 222603作成日:2026年10月26日

Potassium Iodide → HCID 178525739、化合物

https://huagongshe.com/reaction/222603

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium IodideHCID 4875—
反応物Sodium ChlorideHCID 5234—
反応物1,4-DichlorobutaneHCID 8059—
反応物Potassium CarbonateHCID 11430—
反応物HCID 178501209HCID 178501209—
溶媒Acetic AcidHCID 176—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
生成物HCID 178525739HCID 178525739—

反応条件

温度100 °C

反応手順

1,4-Dichlorobutane (2.3 ml, 21 mmol), potassium carbonate (12.6 g, 91 mmol) and potassium iodide (400 mg) are added to a solution of methyl cis-4-aminocyclo-hexanecarboxylate hydrochloride (4 g, 21 mmol) in 32 ml of DMF and the mixture is stirred at 100° C. for 6 h and then at RT for 3 d. The reaction mixture is diluted with 200 ml of water, neutralized with glacial acetic acid, saturated with sodium chloride and extracted with dichloromethane. The organic phases are dried, filtered and evaporated. Yield: 3.8 g of methyl cis-4-(pyrrolidin-1-yl)cyclohexanecarboxylate. The intermediate is then stirred, in 10 ml of methanol, with 25 ml of sodium hydroxide solution (1 N) at RT for 15 h. After the methanol has been removed in vacuo, the reaction mixture is adjusted to pH 6 with hydrochloric acid and evaporated further. The residue is taken up in methanol and purified by filtration through silica gel. Yield: 3.5 g.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08207349B2
出典データセットuspto-grants-2012_06
ORD IDord-f816885f340d4f4c8e5545ee9a3fc62a
出典メモuspto-grants-2012_06