참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetaldehyde | HCID 177 | — |
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 1H-Indole, 1-ethyl-2-methyl- | HCID 170432 | — |
| 반응물 | Sodium p-toluenesulfinate | HCID 2723791 | — |
| 생성물 | [(Methyl)(1-ethyl-2-methyl-3-indolyl)(4-methylphenylsulfonyl)]methane | HCID 20431076 | — |
반응 단계
To a stirred mixture of 175.0 ml of ethyl alcohol, 30.35 g (0.14 mole) of 81.4 percent sodium p-toluenesulfinate, 19.5 g (0.112 mole) of 91.2 percent 1-ethyl-2-methylindole and 5.5 g (0.125 mole) of acetaldehyde under an atmosphere of nitrogen and maintaining the temperature at approximately 5° C. by means of an ice-water bath, there was added dropwise 27.5 ml of concentrated hydrochloric acid. After stirring approximately four hours at ambient temperature, the white solid which had separated was collected by filtration, washed with a small amount of ethyl alcohol and air dried to a constant weight of 43.7 g. The solid was dissolved in a hot mixture of ethyl and methyl alcohols, treated with 3.0 g of decolorizing charcoal, the solution filtered while hot, and then set aside at ambient temperature overnight. The resulting slurry was placed in a refrigerator for approximately two hours. The separated solid was then collected by filtration, washed with 500.0 ml of ethyl alcohol and air-dried to obtain 17.8 g of [(methyl)(1-ethyl-2-methyl-3-indolyl)(4-methylphenylsulfonyl)]methane (Formula X: R=4--CH3 ; R1 =C2H5 ; R2 =CH3 ; R3 =R4 =H; n=1), a pale yellow solid which melted at 140°-142° C. developing a purple color.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04257954 |
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| 출처 데이터셋 | uspto-grants-1981_03 |
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| ORD ID | ord-755d69c262524ec3989f6f32ad2463c2 |
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| 출처 메모 | uspto-grants-1981_03 |
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