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Triethylamine → HCID 57773557、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Isothiocyanatobenzenesulfonamide | HCID 521359 | — |
| 反応物 | 3-Iodobenzylamine hydrochloride | HCID 2723861 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 57773557 | HCID 57773557 | — |
反応手順
To a suspension of 4-isothiocyanatobenzenesulfonamide (378 mg, 1.76 mmol) in dry acetonitrile (10 mL) and triethylamine (0.3 mL, 4.0 mmol) was added 3-iodobenzylamine hydrochloride salt (476 mg, 1.76 mmol). The reaction mixture became warm and a clear solution resulted. After stirring for 2 h the reaction was concentrated and the crude solid recrystallized from methanol/water to afford a white solid. The solid was filtered and washed with hexanes to afford the desired product MIP-1139 (715 mg, 91%). 1H NMR (400 MHz, DMSO-d6) δ 9.95 (br, 1H), 8.48 (br, 1H), 7.74-7.61 (m, 5H), 7.36-7.12 (m, 3H), 4.70 (m, 2H); (M+H)+ (448).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08877970B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-bed49e7bedfa453d8f95e0393c47a205 |
| 出典メモ | uspto-grants-2014_11 |