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Thiophosgene → 2,3-Dimethyl-4-nitrophenyl isothiocyanate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophosgene | HCID 10040 | — |
| 反応物 | 2,3-Dimethyl-4-nitroaniline | HCID 7099035 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2,3-Dimethyl-4-nitrophenyl isothiocyanate | HCID 18316015 | 48% |
反応手順
To a solution of 2,3-dimethyl-4-nitroaniline (0.5 g, 1.0 equiv.) in toluene (50 mL) was added thiophosgene (0.3 mL, 1.3 equiv.) and the reaction mixture was heated at the reflux temp. overnight. The resulting mixture was concentrated under reduced pressure and the residue was purified by column chromatography (25% CH2Cl2/hex) to afford 2,3-dimethyl-4-nitrophenyl isothiocyanate as a light yellow solid (0.30 g, 48%): 1H NMR (CDCl3) δ2.39 (s, 3H), 2.41 (s, 3H), 7.20 (d, J=8.4 Hz, 1H); CI-MS m/z 200 ((M+H)+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06353006B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-d72828e659f34340a7d8282e5173f795 |
| 出典メモ | uspto-grants-2002_03 |