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Triethylamine → 1-Allyl-3-(2,6-dimethylphenyl)-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 | N-Allylglycine | HCID 76651 | — |
| 反応物 | 2,6-Xylyl isothiocyanate | HCID 87976 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Allyl-3-(2,6-dimethylphenyl)-2-thioxo-imidazolidin-4-one | HCID 11414301 | 16.3% |
反応手順
A mixture of N-allyl glycine (17.4 g), 2,6-dimethylphenyl-isothiocyanate (20 g), triethylamine (20.2 g), and methylene chloride (150 mL) was heated at reflux for 3 hours. The reaction mixture was evaporated to dryness. The residual gum was dissolved in diethyl ether, then treated with etheral hydrogen chloride. A white solid formed. The solid was filtered and discarded. The filtrate was concentrated to a residue. The residue was chromatographed on silica gel (CH2Cl2) to give title compound (5.2 g) as an orange solid, m.p. 43°-46° C. Anal. Calcd. for. C14H16N2O S: C, 64.59; H, 6.19; N, 10.76. Found: (2, 64.52; H, 6.08; N, 10.66. Mass spectrum (EI, M.+) m/z 260.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05554607 |
| 出典データセット | uspto-grants-1996_09 |
| ORD ID | ord-b07bece6fde44ec48ba20a8d73c1932d |
| 出典メモ | uspto-grants-1996_09 |