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Ammonium Hydroxide → Methyl[3,5-bis(trifluoromethyl)benzyl][2-cyano-5-(trifluoromethyl)benzyl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Methyl [3,5-bis(trifluoromethyl)benzyl](2-iodo-5-trifluoromethyl-benzyl)carbamate | HCID 59343876 | — |
| 反応物 | HCID 178418546 | HCID 178418546 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl[3,5-bis(trifluoromethyl)benzyl][2-cyano-5-(trifluoromethyl)benzyl]carbamate | HCID 87540861 | — |
反応手順
To a solution of Example 5 dissolved in DMF (1.5 mL) was added CuCN (20 mg, 0.22 mmol) and the resultant mixture was heated at 100° C. for 16 h. The reaction was cooled to room temperature, poured into NH4OH (10 mL) and extracted with EtOAC (4×30 mL). The combined organic extracts were washed with H2O and brine (10 mL each), dried over MgSO4, filtered and concentrated in vacuo. Purification by flash chromatography (0 to 25% EtOAc/hexanes) afforded the title compound as a colorless oil. LCMS=485 (M+1)+. 1H NMR (CDCl3, 500 MHz): δ 7.81 (s, 1H), 7.78 (d, J=7.7 Hz, 1H), 7.67-7.31 (m, 4H), 4.82 (br s, 2H), 4.72 (s, 2H), 3.91 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737295B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-17199744cbc54100870e490b3d461b1f |
| 出典メモ | uspto-grants-2010_06 |