참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-Mercaptoethanol | HCID 1567 | — |
| 반응물 | Bromocycloheptane | HCID 16992 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Hydroxyethyl cycloheptyl sulfide | HCID 22454073 | 92.9% |
반응 단계
2.32 g of 2-mercaptoethanol, dissolved beforehand in 10 cm3 of dimethylformamide, were slowly added, under an inert atmosphere and at a temperature in the region of 20° C., to a stirred suspension of 0.91 g of 60% sodium hydride in 10 cm3 of anhydrous dimethylformamide. After stirring for 20 minutes, 3.5 g of bromocycloheptane, dissolved in 10 cm3 of dimethylformamide, were added. The reaction was brought to completion by stirring at a temperature in the region of 20° C. for 1 hour 30 minutes. The reaction mixture was poured onto 150 cm3 of water to which have been added 100 cm3 of diethyl ether. The ethereal phase was separated by settling and the aqueous phase was extracted once with 50 cm3 of diethyl ether. The organic phases were combined and then washed with 2 times 100 cm3 of water, dried over magnesium sulfate, filtered, and concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 3.2 g of 2-hydroxyethyl cycloheptyl sulfide were obtained in the form of an oil with a yellow color.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06403610B1 |
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| 출처 데이터셋 | uspto-grants-2002_06 |
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| ORD ID | ord-c15893eda1a044219750fd1658c36fda |
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| 출처 메모 | uspto-grants-2002_06 |
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