참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | (1S,2S)-2-amino-3-morpholino-1-phenyl-1-propanol | HCID 10513992 | — |
| 반응물 | 3,6-Dioxadodecanoic acid | HCID 18459613 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | (1S,2S)-2-(3,6-dioxadodecanoyl)amino-3-morpholino-1-phenyl-1-propanol | HCID 69821443 | 47.4% |
반응 단계
Methylene chloride (40 ml), 3,6-dioxadodecanoic acid (1.086 g, 5.325 mmol) and EDC (1.167 g, 6.090 mmol) were added to (1S,2S)-2-amino-3-morpholino-1-phenyl-1-propanol (959.1 mg, 4.064 mmol), followed by stirring for 3 hours. EDC (719.3 mg, 3.752 mmol) was added thereto and the mixture was further stirred for 3 days. After evaporating the solvent under reduced pressure, a saturated sodium hydrogen carbonate solution (70 ml) was added, followed by extraction with ethyl acetate (100 ml). After washed with water (70 ml) and saturated brine (70 ml) successively, the organic layer was dried over sodium sulfate and filtered, and the solvent was evaporated under reduced pressure. The resulting crude product was purified by silica gel column chromatography (chloroform:methanol=30:1) to obtain the title compound (812.3 mg, yield 47.4%) as colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06407064B2 |
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| 출처 데이터셋 | uspto-grants-2002_06 |
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| ORD ID | ord-43d287bbab694ecbb21f02c503f11f47 |
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| 출처 메모 | uspto-grants-2002_06 |
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