참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Butanal | HCID 261 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-Methyl-1,3-dithiane | HCID 22329 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | 2-(1-Hydroxybutyl)-2-methyl-1,3-dithian | HCID 12476960 | — |
반응 단계
56 mmol of n-butyllithium (35 ml of a 1.6 M solution in hexane) were added with stirring to a solution of 2-methyl-1,3-dithian (7 g, 52.1 mmol) in 100 ml of dry tetrahydrofuran at −30° C. under argon. After stirring at −30° C. for 2 hours, the mixture was cooled to −78° C. 4.2 g (58.3 mmol) of freshly distilled n-butyraldehyde were added dropwise in the course of 15 minutes and the mixture was stirred for a further 30 minutes. After warming to 20° C., it was poured into a beaker containing 300 ml of water and 100 ml of n-hexane. The organic phase was separated off and the aqueous phase was extracted three times with 50 ml of dichloromethane in each case. The combined organic phases were washed with 10% strength by weight potassium hydroxide solution, water and concentrated sodium chloride solution, dried over anhydrous sodium sulfate and then distilled. 8.82 g of 2-(1-hydroxybutyl)-2-methyl-1,3-dithian were isolated as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06245328B1 |
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| 출처 데이터셋 | uspto-grants-2001_06 |
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| ORD ID | ord-4a3edc1b5e0642e8be21e20e3154a1ca |
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| 출처 메모 | uspto-grants-2001_06 |
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