関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 5,6-Difluoroisoindoline-1,3-dione | HCID 14818212 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 58136358 | HCID 58136358 | — |
反応手順
740 mg (4.04 mmol) of 5,6-difluoro-1H-isoindole-1,3(2H)-dione were dissolved in 6.6 ml of ethanol, the mixture was cooled to 0° C. and 76.4 mg (2.02 mmol) of sodium borohydride were added a little at a time. After the addition had ended, the reaction mixture was slowly warmed to RT and stirred at RT for another 30 min before the reaction mixture was adjusted to neutral with 1 N hydrochloric acid. The mixture was concentrated to dryness under reduced pressure, and the residue was dried further under high vacuum. This gave 800.8 mg of crude product which was used without further purification for the next reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08987256B2 |
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| 出典データセット | uspto-grants-2015_03 |
|---|
| ORD ID | ord-43d2b618a54049ed9c682d8140125355 |
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| 出典メモ | uspto-grants-2015_03 |
|---|