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5-Chloro-2-methylphenyl isothiocyanate → 2-[3-(5-Chloro-2-methylphenyl)-1-phenyl-thioureido]-acetic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Chloro-2-methylphenyl isothiocyanate | HCID 29519 | — |
| 反応物 | N-Phenylglycine ethyl ester | HCID 75190 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-[3-(5-Chloro-2-methylphenyl)-1-phenyl-thioureido]-acetic acid ethyl ester | HCID 54314562 | 94.9% |
反応手順
A mixture of N-phenyl glycine ethyl ester (8.95 g), 5-chloro-2-methylphenyl-isothiocyanate (9.18 g), and chloroform (200 mL) was heated at reflux for 24 hours. The solvent was evaporated. The residue was crystallized from ethyl acetate/hexane mixture. The solid was collected and dried to give 17.2 g of 2-[3-(5-chloro-2-methylphenyl)-1-phenyl-thioureido]-acetic acid ethyl ester as a white solid, m.p. 148°-1500° C. Anal. Calcd. for. C18H19Cl N2O2S: C, 59.58; H, 5.28; N, 7.72. Found: C, 59.79; H, 5.38; N, 7.65. Mass spectrum (EI, M.+) m/z 262/264.
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-036d5124d7f84efeabd3ccee3b393eec |
| 出典メモ | uspto-grants-1998_10 |