참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | Sodium Thiosulfate | HCID 24477 | — |
| 반응물 | 5,6-Dimethoxyindole | HCID 84431 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-iodo-5,6-dimethoxy-1-methyl-1H-indole | HCID 67147447 | — |
반응 단계
0.465 g of powdered potassium hydroxide is added to a solution of 0.5 g of 5,6-dimethoxy-1H-indole in 15 ml of dimethylformamide. A solution of 0.725 g of bisublimated iodine in 15 ml of dimethylformamide is added dropwise to the above mixture. After agitation of the reaction medium for approximately 3 hours at a temperature in the region of 20° C., 0.21 ml of iodomethane is added dropwise, maintaining the mixture at this same temperature by cooling using a water bath. After agitation at around 20° C. for 1 hour 30 minutes, the mixture is run into a solution of 1.5 g of sodium thiosulfate in 150 ml of water cooled to around 5° C., and agitated for approximately 10 minutes. The precipitate is filter-dried, washed with five times 5 ml of water cooled to around 5° C., and then dried under vacuum (13 kPa) over phosphorus pentaoxide. 0.78 g of 3-iodo-5,6-dimethoxy-1-methyl-1H-indole is obtained in the form of a solid, the characteristics of which are as follows:
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07528147B2 |
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| 출처 데이터셋 | uspto-grants-2009_05 |
|---|
| ORD ID | ord-dc51218fc70f4f84a33c68ed604c49a9 |
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| 출처 메모 | uspto-grants-2009_05 |
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