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Trifluoroacetic acid → TFA acetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 3-Oxo-2-[1(R)-methyl-2(pyridin-2-yl)ethyl]-2,3-dihydro-1-H-isoindole-5-carbonyl-2(S)phenylsulfonylamino-beta-alanine t-butyl ester | HCID 86754267 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | TFA acetonitrile | HCID 21924481 | — |
| 生成物 | Trifluoroacetic acid water | HCID 22392675 | — |
| 生成物 | 3-Oxo-2-[1(R)-methyl-2(pyridin-2-yl)ethyl]-2,3-dihydro-1-H-isoindole-5-carbonyl-2(S)phenylsulfonylamino-beta-alanine | HCID 86754266 | — |
反応手順
A CH2Cl2 solution (20 mL) of 7-7 (44 mg, 0.074 mmol) and TFA (4 mL) was stirred under ambient conditions for 5 h and then concentrated. The residue was azeotroped with toluene (3×25 mL) to give a solid which was purified by HPLC using a VYDAC C18 semiprep column with gradient elution [95:5 (99.9:0.1 H2O/TFA)/(99.9:0.1 CH3CN/TFA)→50:50 (99.9:1 H2O/TFA) (99.9:1 CH3CN/TFA) 60 min] to provide 7-8 as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05925655 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-c25231d2a5f7441f9d9c6ef2c5c1ddf6 |
| 出典メモ | uspto-grants-1999_07 |