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Tetrafluoroboric acid → 4-Hydroxy-1,8-naphthalenedicarboxylic anhydride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrafluoroboric acid | HCID 28118 | — |
| 反応物 | 4-Aminonaphthalene-1,8-dicarboxylic anhydride | HCID 80990 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 4-Hydroxy-1,8-naphthalenedicarboxylic anhydride | HCID 5999497 | 61.6% |
反応手順
To a solution of 1.0 g (4.7 mmol) of 4-amino-1,8-naphthalic anhydride in 5 mL concentrated sulfuric acid at 0° C. to 5° C. was added 1.0 g (14.5 mmol) of sodium nitrite, and then 0.5 mL of water. The reaction was stirred for 30 minutes at 0° C. to 5° C., followed by addition of 5 mL (38 mmol) of 48% aqueous fluoroboric acid, with stirring for 30 minutes. The mixture was poured into ice water. The precipitate was isolated, suspended in a solution of 10 mL concentrated sulfuric acid in 50 mL water, refluxed in 3 hours, and again poured onto ice. The precipitate was isolated, washed with water, and dried to yield 620 mg of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06177423B1 |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-56d8348d4c064626a6e1348ebb805143 |
| 出典メモ | uspto-grants-2001_01 |