化工社化工社 化学情報印刷レポート · 研究参考用
Trityl chloride → 5-Bromo-2-trityl-isoindoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trityl chloride | HCID 6456 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Bromoisoindoline | HCID 14795871 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Bromo-2-trityl-isoindoline | HCID 59263113 | 85.5% |
反応手順
Trityl chloride (2.30 g, 8.23 mmol) was added to a solution of 5-bromo-2,3-dihydro-1H-isoindole (1.64 g, 8.23 mmol) and triethylamine (1.4 mL, 9.9 mmol) in dichloromethane (20 mL). After 18 hours the solvent was removed in vacuo, the residue taken up in ethyl acetate and washed with water (×2) and brine, dried (MgSO4) and concentrated. The crude material was purified by flash chromatography on silica eluting with 1% triethylamine/10% ethyl acetate/petrol to give 5-bromo-2-trityl-2,3-dihydro-1H-isoindole as a reddish-brown solid (3.10 g, 85%). 1H NMR (CDCl3) 7.91-7.84 (1H, m), 7.57 (6H, d), 7.45-7.41 (1H, m), 7.33-7.14 (9H, m), 6.95 (1H, d), 3.90 (2H, s), 3.86 (2H, s). MS: Ph3C+ 243.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08530469B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-a5870101222e4ed58807d3b9eb7901f6 |
| 出典メモ | uspto-grants-2013_09 |