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HRID 1601906作成日:2026年10月26日

Hydrochloric Acid → 5-[2-(4-Anilinopiperid-1-yl)ethyl]-3-[3,5-bis(trifluoromethyl)benzyl]-5-(3,4-dichlorophenyl)-tetrahydro-2H-1,3-oxazin-2-one dihydrochloride monohydrate

https://huagongshe.com/reaction/1601906

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Potassium CarbonateHCID 11430—
反応物4-AnilinopiperidineHCID 89982—
反応物3-[3,5-Bis(trifluoromethyl)benzyl]-5-(3,4-dichlorophenyl)-5-[2-(methanesulfonyloxy)ethyl]tetrahydro-2H-1,3-oxazin-2-oneHCID 15886677—
溶媒WaterHCID 962—
溶媒Diethyl EtherHCID 3283—
溶媒AcetonitrileHCID 6342—
生成物5-[2-(4-Anilinopiperid-1-yl)ethyl]-3-[3,5-bis(trifluoromethyl)benzyl]-5-(3,4-dichlorophenyl)-tetrahydro-2H-1,3-oxazin-2-one dihydrochloride monohydrateHCID 21200476—

反応条件

温度55 °C

反応手順

A mixture of 0.3 g of 4-anilinopiperidine, 0.8 g of the compound obtained in step C of EXAMPLE 4 and 0.69 g of potassium carbonate in 5 ml of acetonitrile is heated at 50-60° C. for 5 hours. The reaction mixture is poured into water and extracted with AcOEt, the organic phase is washed twice with water and with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica H using DCM and then a DCM/MeOH mixture (96/4; v/v) as the eluent. The product obtained is taken up with a saturated solution of gaseous HCl in ether and the precipitate formed is wrung to give 0.12 g of the expected product. M.p.=158° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05977359
出典データセットuspto-grants-1999_11
ORD IDord-410ba793fcef44a796f0d5dcbbb82886
出典メモuspto-grants-1999_11