참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Benzylamine | HCID 7504 | — |
| 반응물 | 1-Chloro-2,3-dihydro-1H-indene | HCID 94465 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2,3-Dihydro-N-benzyl-1H-inden-1-amine | HCID 10130724 | 72.5% |
반응 단계
A mixture of 272 ml of toluene and 199.5 g benzylamine was prepared and heated to 90° C. The chlorindan was added dropwise to the mixture over a 30 minute period. The reaction mixture was heated to 115° C. for ten hours. The reaction mixture was cooled to ambient temperature and 300 ml of water was added. The resulting heterogeneous mixture was then brought to pH2.2 by the addition of 33% H2SO4. The phases were separated and the organic layer discarded. The pH of the aqueous layer was adjusted to pH6.0 prior to extraction with 300 ml of toluene. A further 100 ml of toluene was then added and the aqueous phase discarded. The toluene was removed under vacuo from the combined organic layer leaving 104.3 g racemic N-benzyl-1-aminoindan base as an oil (72.5 % yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06271263B1 |
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| 출처 데이터셋 | uspto-grants-2001_08 |
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| ORD ID | ord-d8bec41e557943cbb1412b80a07156c1 |
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| 출처 메모 | uspto-grants-2001_08 |
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