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S-Trityl-L-Cysteine → HCID 67392281、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | S-Trityl-L-Cysteine | HCID 76044 | — |
| 反応物 | HCID 86626346 | HCID 86626346 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 67392281 | HCID 67392281 | 27.6% |
反応手順
A mixture of trifluoromethanesulfonic acid 2,2-difluoro-1(R)-(4-fluorophenyl)-2-(4-methylsulfanylphenoxy)ethyl ester (1.70 g, 3.8 mmol), 2(R)-amino-3-tritylsulfanylpropionic acid (1.38 g, 38 mmol) and diisiopropylethylamine (2.65 ml, 15.2 mol) in DCM (35 ml) was stirred for 19 h at room temperature. The solvent was evaporated under vacuum and the residue dissolved in ethyl ether (20 ml). The solution was washed with 1N HCl solution and brine. After drying over sodium sulfate, the solvent was evaporated and the crude was purified by flash chromatography, using a mixture of EA/H (1/3) as eluent to give 2(R)-[2,2-difluoro-1(S)-(4-fluorophenyl)-2-(4-methylsulfanylphenoxy)ethylamino]-3-tritylsulfanylpropionic acid (0.693 g, 27%) as a foam.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08013186B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-4a6238a676b54927aebafa69272d91a4 |
| 出典メモ | uspto-grants-2011_09 |