참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Chloro-N,N,N',N'-tetramethylformamidinium Hexafluorophosphate | HCID 10989639 | — |
| 반응물 | 1-(4-methoxybutyl)-7-oxo-4,5,6,7-tetrahydro-1H-indole-2-carboxylic acid | HCID 58355389 | — |
| 반응물 | tert-Butyl (3S,5R)-3-(isobutylamino)-5-(morpholine-4-carbonyl)piperidine-1-carboxylate | HCID 59356577 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 용매 | Sodium Bicarbonate | HCID 516892 | — |
| 생성물 | HCID 58355174 | HCID 58355174 | 50.3% |
반응 단계
1-(4-Methoxybutyl)-7-oxo-4,5,6,7-tetrahydro-1H-indole-2-carboxylic acid (210 mg), tert-butyl (3S,5R)-3-[(2-methylpropyl)amino]-5-(morpholin-4-ylcarbonyl)piperidine-1-carboxylate (292 mg) and N,N-diisopropylethylamine (550 μl) were dissolved in 1,2-dichloroethane (10 ml), chloro-N,N,N′,N′-tetramethylformamidinium hexafluorophosphate (244 mg) was added, and the mixture was stirred at room temperature for 15 hr. The reaction mixture was diluted with saturated aqueous sodium hydrogen carbonate solution and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate-hexane (10:90-100:0) was concentrated under reduced pressure to give the object product (245 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08664380B2 |
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| 출처 데이터셋 | uspto-grants-2014_03 |
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| ORD ID | ord-d1ae4f34dbd14d1a80280c73fb0df70d |
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| 출처 메모 | uspto-grants-2014_03 |
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