참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Thiophene | HCID 8030 | — |
| 반응물 | Tin tetrachloride | HCID 24287 | — |
| 반응물 | Hexanoyl chloride | HCID 67340 | — |
| 용매 | Benzene | HCID 241 | — |
| 생성물 | 2-Hexanoylthiophene | HCID 520264 | 77.2% |
반응 단계
In a 5 liter-five-necked flask, 187.3 g (2.23 mol) of thiophene, 300 g (2.23 mol) of n-hexanoyl chloride and 2.7 liter of dry benzene were placed and cooled below 0° C. To the mixture under stirring, 237.9 g (9.13×10-1 mol) of SnCl4 was added dropwise in 1 hour below 0° C. The mixture was stirred for 30 min. below 0° C., followed by stirring for 3.5 hours while being gradually restored to room temperature. After the reaction, 2 liter of 10% HCl was added to the reaction mixture, followed by stirring for 10 min. The separated organic layer was successively washed three times with 500 ml each of 10% HCl, water, 5% Na2CO3 and water, followed by drying with CaCl2 and distilling-off of the solvent to obtain 408 g of a crude product. The crude product was subjected to reduced-pressure distillation in an atmosphere of nitrogen to obtain 313.4 g of a pure product (yield: 77.2%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05118441 |
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| 출처 데이터셋 | uspto-grants-1992_06 |
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| ORD ID | ord-fcff1cf7fcc44bcda8503cbcc30ee44a |
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| 출처 메모 | uspto-grants-1992_06 |
|---|