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4-Hydrazinobenzenesulfonic acid → 6-(2,3-dimethyl-5-sulfo-3H-indol-3-yl)hexanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Hydrazinobenzenesulfonic acid | HCID 66825 | — |
| 反応物 | 7-Methyl-8-oxononanoic acid | HCID 22266823 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 6-(2,3-dimethyl-5-sulfo-3H-indol-3-yl)hexanoic acid | HCID 59855422 | — |
反応手順
4-Hydrazinobenzenesulfonic acid (1.88 g, 10 mmol), 7-methyl-8-oxononanoic acid (2.8 g, 15 mmol) and glacial acetic acid (10 ml) were mixed and heated under reflux for 6 hrs. The solvent was then evaporated under vacuum and the residue triturated with diethyl ether until a solid was obtained. This was dried under vacuum to give crude product, 3.4 g (100%). This was purified by preparative HPLC as required (RPC18. Water+0.1% TFA→MeCN+0.1% TFA gradient). UV/Vis (Water+0.1% TFA): 274, 229, 204 nm. 1H-nmr (D2O) δ 0.6-0.9 (2H, broad m), 1.10-1.25 (2H, broad m), 1.35-1.50 (2H, m), 1.60 (3H, s), 2.10-2.40 (2H, broad m+2H, t), 7.77 (1H, d), 7.97 (1H, dd) and 8.06 (1H, d)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08044203B2 |
| 出典データセット | uspto-grants-2011_10 |
| ORD ID | ord-686d6b4543cf441880c75b51e59452c7 |
| 出典メモ | uspto-grants-2011_10 |