참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | Isobutyl chloroformate | HCID 62365 | — |
| 반응물 | 2-(9H-fluoren-9-ylmethoxycarbonylamino)-3-[4-[(2-methylpropan-2-yl)oxy]phenyl]propanoic acid | HCID 100112 | — |
| 반응물 | HCID 178420112 | HCID 178420112 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178450149 | HCID 178450149 | 88.2% |
반응 단계
3-(4-tert-Butoxy-phenyl)-2-(9H-fluoren-9-ylmethoxycarbonylamino)-propionic acid (1.93 g, 4.2 mmol) was dissolved in dichloromethane (100 mL), cooled to 0° C., then N-methyl-morpholine (0.42 g, 4.2 mmol) was added neat followed by isobutyl chloroformate (0.52 mL, 4 mmol). After 1.25 hour 3-(4-phenyl-1H-imidazol-2-yl)-1,2,3,4-tetrahydro-isoquinoline (1.10 g, 4 mmol) was added neat and the reaction was allowed to warm to room temperature. After 16 hours the reaction was extracted with water, then saturated NaHCO3, dried over Na2SO4, filtered, and concentrated under reduced pressure to give 2.53 g (88%) of brown foam desired product {1-(4-tert-butoxy-benzyl)-2-oxo-2-[3-(4-phenyl-1H-imidazol-2-yl)-3,4-dihydro-1H-isoquinolin-2-yl]-ethyl}-carbamic acid 9H-fluoren-9-ylmethyl ester, which was used without further purification. (LC/MS; Measured MW (MH+): 717)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07202381B2 |
|---|
| 출처 데이터셋 | uspto-grants-2007_04 |
|---|
| ORD ID | ord-5dd0378a82ec4e4fa6630b9b477abd5f |
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| 출처 메모 | uspto-grants-2007_04 |
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