関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Tritylamine | HCID 138598 | — |
| 反応物 | 1,2-Bis(bromomethyl)-4-iodobenzene | HCID 66726722 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Iodo-2-tritylisoindoline | HCID 66726248 | 48% |
反応手順
A mixture of the product of Step B (0.34 g; 0.87 mmol) hydrochloride salt of tritylamine (0.22 g; 0.87 mmol) and N,N-diisopropylethylamine (DIPEA) (0.49 ml; 2.8 mmol) in anhydrous DMF (3 ml) was stirred for 2 h at 60° C. under N2. After removing the solvent in vacuo, the residue was diluted to 15 ml with ethyl acetate (EtOAc) and washed with, H2O, brine and dried over anhydrous MgSO4 and filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was purified by FCC (SiO2; hexane/EtOAc, 8:2) to give pure title compound (0.2 g; 48%) as colourless heavy syrup. 1H-NMR (CDCl3) 3.86 (s, 2H); 3.87 (s, 2H); 6.81-7.57 (m, 18H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09181182B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-2b25a432ae864e688dac041a97b72a02 |
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| 出典メモ | uspto-grants-2015_11 |
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