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Hydrochloric Acid → o-(4-Hydroxyphenyl)-3,5-diiodo-l-tyrosine methyl ester
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; 4.8 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. (1949), 3424-3433) in MeOH (12 was stirred for 4 days at 20° C. Then a NaHCO3 saturated aqueous solution was added to the mixture until pH 7 was reached, obtaining a precipitate which was filtered by concentration of the solution a second crop of precipitate was obtained. The two samples were combined and dried (50° C.; 1.3 kPa) 3.7 mmol). Yield 87%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06458337B1 |
| 出典データセット | uspto-grants-2002_10 |
| ORD ID | ord-63772df48e1d40cdb38e7b6a1d3b5bff |
| 出典メモ | uspto-grants-2002_10 |