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HRID 2172896作成日:2026年10月25日

Chloroform → 4-Chloro-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-2-amine

https://huagongshe.com/reaction/2172896

反応式

関与物質

役割名称HCID仕込み量
反応物ChloroformHCID 6212—
反応物HexaneHCID 8058—
反応物Phosphorus oxychlorideHCID 24813—
反応物2-Amino-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4(3h)-oneHCID 290197—
溶媒Acetic AnhydrideHCID 7918—
生成物4-Chloro-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-2-amineHCID 1291020044%

反応手順

To a 50 mL flask was added 10 (221 mg, 1 mmol) and 10 mL POCl3. The resulting mixture was refluxed for 2 h, and the solvent was removed under reduced pressure to afford a dark residue. To this was added 30 mL of CHCl3 and 300 mg of silica gel. The solvent was evaporated to afford a plug. Column chromatography of the plug with hexane: acetyl acetate=20:1 as eluent afford 105 mg (44%) of 11 as a yellow solid:

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09056869B2
出典データセットuspto-grants-2015_06
ORD IDord-4357a1e6bed444b79c90c45b72e89348
出典メモuspto-grants-2015_06