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Pyridine → N-benzyl-N'-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Benzyl isocyanate | HCID 76639 | — |
| 反応物 | 2-(4-Aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol | HCID 577801 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-benzyl-N'-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}urea | HCID 44968109 | 75% |
反応手順
Into a 4 mL vial is added 2-(4-aminophenyl)-1,1,1,3,3,3-hexafluoro-2-propanol (75 mg, 0.289 mmol), anhydrous pyridine (1 mL) and benzyl isocyanate (0.036 mL, 0.289 mmol). The reaction mixture was stirred at r.t. for 2 days. To the reaction mixture is added H2O to precipitate the product. The solid is filtered and purified by preparative TLC (MeOH/CHCl3 10:90) to give a colorless solid (84.3 mg, 75%). m.p. 163-164° C. (dec). 1H NMR (DMSO & CHCl3) 4.23 (d, 2H), 6.05 (t, 1H), 7.05 (m, 1H), 7.08 (m, 4H), 7.25 (t, 3H), 7.42 (d, 2H), 8.02 (s, 1H); ESIMS: m/z 393 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07385063B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-245a48fac34b48daa90291c5d4532eca |
| 出典メモ | uspto-grants-2008_06 |