참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 반응물 | 1-Benzyl-2-piperidone | HCID 5170076 | — |
| 반응물 | 2-(5-Methoxy-2-nitrophenyl)ethan-1-amine | HCID 18621975 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | (1-Benzylpiperidin-4-yl)-[2-(5-methoxy-2-nitrophenyl)-ethyl]-amine | HCID 21109931 | 100% |
반응 단계
Under a nitrogen atmosphere a mixture of 9.98 g (50.9 mmol) 2-(5-methoxy-2-nitrophenyl)-ethylamine, 9.80 mL (54.9 mmol) N-benzylpiperidone and 6.30 mL (114 mmol) acetic acid in 270 mL DCM was cooled to 0° C. in an ice bath. At this temperature 14.2 g (67.0 mmol) sodium triacetoxyborohydride were added batchwise within 20 min. The reaction mixture was stirred for a further 4 h at 0° C. and left to warm up to RT overnight. Then the mixture was combined with 400 mL of a 15% (w/v) aqueous potassium carbonate solution and stirred for 1 h at RT. The organic phase was separated off, dried and concentrated by rotary evaporation. 18.8 g of the desired product were obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08629137B2 |
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| 출처 데이터셋 | uspto-grants-2014_01 |
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| ORD ID | ord-3e1c2f221c9e4506885fd66d5bd83c5b |
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| 출처 메모 | uspto-grants-2014_01 |
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