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Triethylamine → 3-(5-Chloro-2-methylphenyl)-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 | 5-Chloro-2-methylphenyl isothiocyanate | HCID 29519 | — |
| 反応物 | Ethyl N-methylaminoacetate hydrochloride | HCID 171173 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 3-(5-Chloro-2-methylphenyl)-1-methyl-2-thioxo-imidazolidin-4-one | HCID 18968209 | 72.3% |
反応手順
A mixture of sarcosine ethyl ester hydrochloride (7.68 g), 5 -chloro-2-methylphenyl-isothiocyanate (9.18 g), triethyl amine (12 g) and chloroform (200 mL) was heated at reflux for 5 hours. The mixture was cooled to ambient temperature, washed with 1N HCl(2×200 ), then with water (200 mL) The organic phase was evaporated to dryness. The residue was crystallized from ethanol to give the tide compound (9.2 g) as a tan solid, m.p. 132°-134° C. Anal. Calcd. for C11H11 Cl N2O S: C, 51.87; H, 4.35; N,11.00. Found: C, 51.79; H, 4.12; N, 10.73. Mass spectrum (EI, M.+) m/z 254/256.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05821372 |
| 出典データセット | uspto-grants-1998_10 |
| ORD ID | ord-e0a61f638d964b3fb6a7b8356074f46f |
| 出典メモ | uspto-grants-1998_10 |