関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Thyroxine | HCID 5819 | — |
| 反応物 | 3,5-Diiodothyronine, L- | HCID 92859 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | o-(4-Hydroxyphenyl)-3,5-diiodo-l-tyrosine methyl ester | HCID 14011739 | 87% |
反応手順
A 6 M solution of HCl in MeOH (8 mL; 48 mmol) was added to a suspension of O-(4-hydroxyphenyl)-3,5-diiodo-L-tyrosine (2.12 g; 5 mmol) (prepared according to: Chalmers J. R., Dickson G. T., Elks J. and Hems D. A., “The Synthesis of Thyroxine and Related Substances”, Part V., J. Chem. Soc., 3424-3433, 1949) in MeOH (12 mL). The resulting solution was left under stirring for 4 days at 20° C. Then an NaHCO3 aqueous saturated solution was added until pH 7, to obtain a precipitate which was filtered. After concentration of the solution, a second amount of precipitate was obtained. The two samples were combined and dried (50° C.; 1.3 kPa), to, give the desired product (2 g; 3.7 mmol). Yield 87%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06337064B1 |
|---|
| 出典データセット | uspto-grants-2002_01 |
|---|
| ORD ID | ord-dbaea7d70c82471d8e3fd105c3f4713f |
|---|
| 出典メモ | uspto-grants-2002_01 |
|---|