Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → L-Thyronine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Iodine, ion (I1+) | HCID 3715291 | — |
| 반응물 | N-Trifluoroacetyl-3,5-diiodotyrosine methyl ester | HCID 13941953 | — |
| 반응물 | Diazabicyclo[5.4.0]undecane | HCID 21921200 | — |
| 생성물 | L-Thyronine | HCID 5461103 | 4% |
반응 단계
N-Trifluoroacetyl-3,5-diiodotyrosine methyl ester (552 mg, 1.0 mmol) prepared according to the procedure of N. Lewis and P. Wallbank, Synthesis 1103 (1987) (incorporated by reference) and all of the crude iodonium salt (3) from above is dissolved in 5 mL of anhydrous methanol. Diazabicyclo[5.4.0]undecane (DBU) (183 mg, 1.2 mmol) and a spatula tip of copper-bronze are added and the resulting mixture is stirred at room temperature overnight. The next day, the reaction mixture is filtered, and the filtrate is concentrated in vacuo. The crude residue is purified by flash chromatography (silica gel, 10% ethyl acetate/hexane) to provide 30 mg (4%) of the protected thyronine adduct (4).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06236946B1 |
| 출처 데이터셋 | uspto-grants-2001_05 |
| ORD ID | ord-4cf6c81fbd79408cbdbd8eabaabafd0b |
| 출처 메모 | uspto-grants-2001_05 |