참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Methylbenzenethiol | HCID 7811 | — |
| 반응물 | Ethyl dichloroacetate | HCID 10808 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | Ethyl 2,2-bis(4-methylthiophenoxy)acetate | HCID 13107767 | 68% |
반응 단계
Sodium (3.54 g) is dissolved in methanol (140 cc) and a solution of 4-methylthiophenol (21.8 g) in methanol (25 cc) is added. The mixture is stirred for 1 hour at 20° C. and a solution of ethyl dichloroacetate (12.5 g) in methanol (30 cc) is then added. The mixture is allowed to cool, the white precipitate obtained is filtered off, and the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C. The oil obtained is taken up in diethyl ether (250 cc) and washed four times with N sodium hydroxide solution (50 cc each time) and four times with distilled water (50 cc each time). The ethereal phase is dried over anhydrous sodium sulphate, filtered, treated with animal charcoal, filtered and concentrated to dryness under reduced pressure (20 mmHg) at 40° C. Ethyl 2,2-bis(4-methylthiophenoxy)acetate (18 g) is thus obtained as a yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04225589 |
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| 출처 데이터셋 | uspto-grants-1980_09 |
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| ORD ID | ord-6bb31a9cb3cd4b5eaac488e1d6f003df |
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| 출처 메모 | uspto-grants-1980_09 |
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