関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Perfluorobutanesulfonic acid | HCID 67815 | — |
| 反応物 | Iodonium, diphenyl-, bromide (1:1) | HCID 73871 | — |
| 触媒 | Silver(II) oxide | HCID 92152 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Diphenyliodanium nonafluorobutane-1-sulfonate | HCID 16216934 | 79.3% |
反応手順
To 100 ml of methanol, 3.61 g (0.01 mole) of diphenyliodonium bromide and 1.62 g (0.007 mole) of silver oxide were suspended, then the mixture was reacted at room temperature for 2 hours. To the reaction solution, 4.2 g (0.014 mole) of nonafluorobutanesulfonic acid was added drop-wise at room temperature, followed by reacting at the same temperature for 2 hours while stirring. The thus obtained reaction mixture was filtered and concentrated under reduced pressure, followed by purifying 6.4 g of the residue by column chromatography [Wako gel, C-200; eluent of methylene chloride/methanol=9/1 (v/v)], to obtain 4.6 g of diphenyliodonium nonafluorobutanesulfonate as a colorless crystal. The thus obtained crystal was named acid generator B1. The measurement results of melting point and NMR of acid generator B1 are shown bellow.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07312014B2 |
|---|
| 出典データセット | uspto-grants-2007_12 |
|---|
| ORD ID | ord-6c2008237a64455bb97166bc766e048d |
|---|
| 出典メモ | uspto-grants-2007_12 |
|---|