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Triethylamine → 2-Tert-butoxy-2-(1-(4-chlorophenyl)-3-methyl-7-vinylnaphthalen-2-yl)acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Tributylvinyltin | HCID 81998 | — |
| 反応物 | Ethyl 2-(7-bromo-1-(4-chlorophenyl)-3-methylnaphthalen-2-yl)-2-tert-butoxyacetate | HCID 67126201 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | 2-Tert-butoxy-2-(1-(4-chlorophenyl)-3-methyl-7-vinylnaphthalen-2-yl)acetic acid | HCID 56599936 | — |
反応手順
2-tert-Butoxy-2-(1-(4-chlorophenyl)-3-methyl-7-vinylnaphthalen-2-yl)acetic acid (76) was prepared by the method of Example 67 from ethyl 2-(7-bromo-1-(4-chlorophenyl)-3-methylnaphthalen-2-yl)-2-tert-butoxyacetate using tributyl(vinyl)tin and without triethylamine. 1H-NMR: 400 MHz, (CD3OD) δ: 7.74 (d, J=9 Hz, 1H), 7.65 (m, 2H), 7.55 (m, 3H), 7.32 (d, J=9 Hz, 1H), 7.13 (s, 1H), 6.65 (dd, J=18, 11 Hz, 1H), 5.71 (d, J=18 Hz, 1H), 5.19 (d, J=11 Hz, 1H), 5.17 (s, 1H), 2.59 (s, 3H), 0.98 (s, 9H). HPLC (Kinetex 2.6u, 50×4.6 mm, 2-100% MeCN/H2O+0.05% HOAc, 5 min run): tR (min)=3.99.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09102614B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-64c72200eb2349e1affaae77df688129 |
| 出典メモ | uspto-grants-2015_08 |