참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Nitrobenzaldehyde | HCID 11101 | — |
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | 1-Benzylpiperidin-4-amine dihydrochloride | HCID 12594483 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 1-Benzyl-4-[N-(o-nitrobenzyl)-amino]-piperidine dihydrochloride | HCID 13051019 | 73.1% |
반응 단계
In this reference example, 5.24 g of 1-benzyl-4-amino-piperidine dihydrochloride, 3.02 g of o-nitrobenzaldehyde, 2.02 g of triethylamine and 30 ml of methanol are mixed and stirred at room temperature for one hour. The resultant solution is cooled with ice and stirred. To the stirred solution, 1 g of sodium borohydride is added little by little over a period of one hour. Then, the mixture is brought back to room temperature and stirred at room temperature for 2 hours. The resultant solution is poured into 200 ml of ice water and extracted with ether. The organic layer is washed with water, dried and concentrated. The oily residue is dissolved in 20 ml of ethanol. The solution is mixed with 10 ml of a solution of 5.7 N hydrochloric acid in ethyl acetate. The white crystals deposited are separated by filtration, washed with 20 ml of ethyl acetate and dried to obtain 5.70 g of a crude product. The crude product is recrystallized from hot ethanol to obtain 2.90 g of the desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04344945 |
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| 출처 데이터셋 | uspto-grants-1982_08 |
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| ORD ID | ord-619d1ae7e2054bb8a316ed4a01e897db |
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| 출처 메모 | uspto-grants-1982_08 |
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