참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trityl chloride | HCID 6456 | — |
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Butene-1,4-diol, (2Z)- | HCID 643790 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Trityloxy-but-2-en-1-ol | HCID 54110411 | 85.2% |
반응 단계
Trityl chloride (557 mg; 2 mmol) Et3N (0.306 ml; 2.2 mmol) and DMAP (10 mg; 0.08 mmol) were added to an emulsion of cis-2-buten-1,4-diol (1.76 g; 20 mmol) in DCM (10 ml). The mixture was stirred at room temperature under atmosphere of nitrogen for 24 hours. After such period of time the complete disappearance of trityl chloride was observed by TLC (EtOAC/Hexane 50:50). DCM (20 ml) and water (10 ml) were added to the mixture. The phases were separated and the organic layer was washed with water (10 ml) and brine (10 ml). The solvent was dried over MgSO4 and evaporated under reduced pressure affording a residue (white oil) which was purified by flash chromatography using Hexane/EtOAc 70:30→40:60 as gradient which gave the title product as a colourless oil (563 mg, 81%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08017620B2 |
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| 출처 데이터셋 | uspto-grants-2011_09 |
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| ORD ID | ord-7ed79087e5734d59be9aaab4b8664e48 |
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| 출처 메모 | uspto-grants-2011_09 |
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