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Methanol → Methyl 6,7,8,9-tetrahydropyrido[1,2-a]indole-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | 6,7,8,9-Tetrahydropyrido[1,2-a]indole | HCID 10855942 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 6,7,8,9-tetrahydropyrido[1,2-a]indole-1-carboxylate | HCID 19778122 | 70.3% |
反応手順
6,7,8,9-tetrahydropyrido[1,2-a]indole (1.15 g, 6.7 mmol) in methylene chloride (5 ml) was added dropwise at 0° C. to a solution of phosgene (10 mmol) in toluene (5 ml). The reaction mixture was stirred for one hour after which methanol (1 ml) was added gradually and the mixture allowed to warm to ambient temperature. The solvent was removed under reduced pressure to yield a white solid. Recrystallization from hexane afforded 1.08 g (70.3% of methyl 6,7,8,9-tetrahydropyrido[1,2-a]indole-1-carboxylate, as white crystals, m.p. 102°-103° C. Anal. for C14H15NO2 : Calcd. C, 73.34; H, 6.59; N, 6.11. Found: C, 72.96; H, 6.61; N, 6.33.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05189041 |
| 出典データセット | uspto-grants-1993_02 |
| ORD ID | ord-ba37bc30eb764beab3f6b6c46c68ea25 |
| 出典メモ | uspto-grants-1993_02 |