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1-Chloroethyl chloroformate → 3-(4-Isopropylphenyl)-4,6,7-trimethylspiro[benzofuran-2(3h),4'-piperidine]hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Chloroethyl chloroformate | HCID 521305 | — |
| 反応物 | 1'-Benzyl-3-(4-isopropylphenyl)-4,6,7-trimethylspiro[benzofuran-2(3H), 4'-piperidine] | HCID 21961343 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(4-Isopropylphenyl)-4,6,7-trimethylspiro[benzofuran-2(3h),4'-piperidine]hydrochloride | HCID 21961353 | 81.3% |
反応手順
To a solution of 1′-benzyl-3-(4-isopropylphenyl)-4,6,7-trimethylspiro[benzofuran-2(3H),4′-piperidine] (10.26 g, 23.34 mmol) in tetrahydrofuran (100 ml) was added α-chloroethyl chloroformate (3.76 g, 26.60 mmol) and the resulting mixture was refluxed with heating for 1 hour. The reaction mixture was cooled down to room temperature and concentrated under reduced pressure. Methanol (80 ml) was added into the resulting residue and the mixture was refluxed for 1 hour. The reaction mixture was cooled down to room temperature and concentrated under reduced pressure. The residue was crystallized from ethanol to obtain 7.32 g (81% yield) of the title compound. Melting point: >260° C. (decomposed).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06479536B1 |
| 出典データセット | uspto-grants-2002_11 |
| ORD ID | ord-3d13394c921f491b90b526fdfb779109 |
| 出典メモ | uspto-grants-2002_11 |