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4-Bromoanisole → 3,5-Di-(tert-butyldimethylsilyloxy)-4'-methoxybenzhydrol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Bromoanisole | HCID 7730 | — |
| 反応物 | 3,5-Bis(tert-butyldimethylsilyloxy)benzaldehyde | HCID 10915545 | — |
| 生成物 | 3,5-Di-(tert-butyldimethylsilyloxy)-4'-methoxybenzhydrol | HCID 11145198 | 82% |
反応手順
Combining 4-bromoanisole (0.43 g) and aldehyde 9a (0.76 g) provided 3,5-di-(tert-butyldimethylsilyloxy)-4′-methoxybenzhydrol 15d as a faint yellow oil (0.80 g, 82%): EIMS m/z 474 (M+), 459, 417, 361, 343, 73; IR (KBr, cm−1) νmax 3420, 2932, 2859, 2361, 1591, 1451, 1252, 1163, 1026, 833; 1H-NMR δ 7.29 (2H, d, J=9.04 Hz), 6.89 (2H, d, J=9.0 Hz), 6.52 (2H, d, J=2.0 Hz), 6.28 (1H, t, J=2.0 Hz), 5.70 (1H, s), 3.83 (3H, s, OCH3), 1.00 (18H, s, C(CH3)3×2), 0.20 (12H s, Si(CH3)2×2); 13C-NMR (75.5 MHz) δ 159.0, 156.5, 146.1, 136.0, 127.9, 113.7, 111.5, 111.0, 75.5, 55.3, 25.7, 18.2, −4.4. Anal. (C26H42O4Si2) C, H.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07705188B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-0d1cdd71fe134984adff59778e1506f5 |
| 出典メモ | uspto-grants-2010_04 |