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HRID 714067作成日:2026年10月25日

Methanol → HCID 71811365、化合物

https://huagongshe.com/reaction/714067

反応式

関与物質

役割名称HCID仕込み量
反応物MethanolHCID 887—
反応物Acetyl chlorideHCID 6367—
反応物TriethylamineHCID 8471—
反応物4-(8-Amino-5,6,7,8-tetrahydro-4-isoquinolinyl)benzonitrileHCID 71811360—
溶媒DichloromethaneHCID 6344—
生成物HCID 71811365HCID 7181136544%

反応手順

A cooled (−20° C.) solution of (rac)-4-(8-amino-5,6,7,8-tetrahydroisoquinolin-4-yl)benzonitrile (example 1) (62.3 mg, 250 μmol) in CH2Cl2 (3.6 ml) was treated with acetyl chloride (21.3 μL, 275 μmol) and Et3N (41.8 μL, 300 μmol). After ½ h, an additional drop of acetyl chloride was added and after 5 min. the mixture was treated with MeOH (0.2 mL) and extracted with water/AcOEt (3×). The organic phases were dried over Na2SO4, filtered and evaporated under reduced pressure. Purification by flash chromatography (50 g SiO2, Telos-cartridge, CH2Cl2/MeOH (2 to 3%)) and precipitation from CH2Cl2 with n-pentane gave the title compound (32 mg, 44%) as off-white powder. MS: 292.1 (M+H+).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09187429B2
出典データセットuspto-grants-2015_11
ORD IDord-b3f37c8c20a84311889dc85bf9c358c3
出典メモuspto-grants-2015_11