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Methanol → Methyl 11-bromoundecanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 11-Bromoundecanoic acid | HCID 17812 | — |
| 反応物 | Calcium Chloride | HCID 5284359 | — |
| 生成物 | Methyl 11-bromoundecanoate | HCID 223913 | 84% |
反応手順
11-Bromoundecanoic acid (commercial material, 25.0 g, 94 mmol), Duolite H+ resin (10 g), calcium chloride (26.2 g, 94 mmol) and methanol (700 ml) were stirred for 15 h. The methanol was removed and dichloromethane was added. The mixture was washed with water, dried (Na2SO4) and concentrated. Distillation gave pure 103 (22.0 g, 84%) with b.p. 103°-104° (2×10-2 torr). 1H-NMR (CDCl3, Me4Si) δ 3.67 (s, 3H, MeO), 3.41 (t, 2H, J=6.8 Hz, Br--CH2), 2.31 (t, 2H, J=7.3 Hz, CH2CO).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04675392 |
| 出典データセット | uspto-grants-1987_06 |
| ORD ID | ord-602b2bdb47f54c15b743da6bba95f29f |
| 出典メモ | uspto-grants-1987_06 |