関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | 6-Bromo-3,4-dihydro-2H-isoquinolin-1-one | HCID 21865450 | — |
| 試薬 | Potassium tert-butoxide | HCID 23665647 | — |
| 触媒 | Binap, (A+-)- | HCID 634876 | — |
| 触媒 | Palladium (II) acetate | HCID 4144353 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-benzylamino-3,4-dihydro-2H-isoquinolin-1-one | HCID 67223915 | 0% |
反応手順
**Repeat 02915-84 but use MW* only. Reduce benzylamine from 4 to 2 eqs.** In a 10 mL sealed MW* test tube was 6-bromo-3,4-dihydroisoquinolin-1(2H)-one (100 mg, 0.44 mmol), phenylmethanamine (97 µl, 0.88 mmol), BINAP (13.77 mg, 0.02 mmol) and palladium(II) acetate (4.97 mg, 0.02 mmol) in DMF (500 mL) combined to give a tan suspension. potassium tert-butoxide (49.6 mg, 0.44 mmol) was then added last. Placed test tube onto Smith MW* platform. Heated reaction to 130°C for 15 minutes. Reaction know a cloudy pale amber. Took LCMS - there is NO product present, ALL SM!!! Placed sealed test tube in heated (130°C) oil bath over weekend. Took LCMS - all SM is consumed but NO desired product is seen!!! Discarded reaction.
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
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| ORD ID | ord-77ff9a88bff94b57b6f8498de8922bdf |
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| 出典メモ | 750 AstraZeneca ELN dataset |
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