참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Borane;tetrahydrofuran | HCID 2723981 | — |
| 반응물 | 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one | HCID 11401769 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride | HCID 22004098 | — |
반응 단계
22.13 g (100 mmol) of the product obtained in Step 1, suspended in 250 mL of THF, are cooled to 0° C. There are then added, dropwise, over 15 minutes, 250 mL of borane/THF (1M in the THF) and heating is carried out at 80° C. for 24 hours. Cooling is carried out and there are then added, dropwise, 250 mL of ethanol, and then 2.6N ethanolic HCl. Heating at reflux is carried out for 40 minutes; some light insoluble material is filtered off and evaporation to dryness is carried out. The residue thereby obtained is recrystallised from a mixture of 150 mL of isopropanol and 20 mL of water to yield the desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08076325B2 |
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| 출처 데이터셋 | uspto-grants-2011_12 |
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| ORD ID | ord-36f8f94c5ab04e7ea8422c96ea1e1876 |
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| 출처 메모 | uspto-grants-2011_12 |
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