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Triethylamine → 3-(Indan-5-yl)-1-methyl-2-thioxo-imidazolidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl N-methylaminoacetate hydrochloride | HCID 171173 | — |
| 反応物 | 5-isothiocyanato-2,3-dihydro-1H-indene | HCID 2759357 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 3-(Indan-5-yl)-1-methyl-2-thioxo-imidazolidin-4-one | HCID 11195962 | 73.5% |
反応手順
A mixture of sarcosine ethyl ester hydrochloride (6.7 g), indan-5-yl-isothiocyanate (7.7 g), triethyl amine (12 g) and chloroform (300 mL) was heated at reflux for 5 hours. The mixture was cooled to ambient temperature, washed with 1N HCl (2×200 mL) then with water (200 mL) The organic phase was evaporated to dryness. The residue was crystallized from ethyl acetate to give the title compound (7.9 g) as a tan solid, m.p. 158°-160° C. Anal. Calcd. for C13H14N2OS: C, 63.39; H, 5.73; N, 11.37. Found: C, 63.30; H, 5.81; N, 11.31. Mass spectrum (EI, M.+) m/z 246.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05861517 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-03b3ef41938641d5ae8165737657860c |
| 出典メモ | uspto-grants-1999_01 |