참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Chlorotrimethylsilane | HCID 6397 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | beta-Chloropivalic acid | HCID 83542 | — |
| 반응물 | Sodium beta-chloropivalate | HCID 23670066 | — |
| 반응물 | Benzenecarbothioic acid, sodium salt (1:1) | HCID 23688990 | — |
| 반응물 | HCID 178526132 | HCID 178526132 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 178446918 | HCID 178446918 | — |
반응 단계
To a solution of sodium β-chloropivalate, prepared from β-chloropivalic acid (13.66 g) and 50% sodium hydride (4.80 g) in dimethylformamide (110 ml) was added dropwise trimethyl chlorosilane (10.85 g) in dimethylformamide (10 ml) at -5° C. to -3° C. After stirring for 1 hour sodium thiobenzoate, prepared from thiobenzoic acid (13.8 g) and 50% sodium hydride (4.80 g) in dimethylformamide (70 ml), was added dropwise thereto at -5° C. to -8° C. After addition of sodium iodide (15.0 g), the mixture was stirred at room temperature for 3 days and then at 40° C. for 7 days. The reaction mixture was diluted with ice-water and extracted with ethyl acetate. The ethyl acetate extract was washed with water, dried over anhydrous sodium sulfate and evaporated in vacuo. The residue was recrystallized from diisopropyl ether-petroleum ether to give β-benzoylthiopivalic acid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04742052 |
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| 출처 데이터셋 | uspto-grants-1988_05 |
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| ORD ID | ord-a73e3a68e2864043b4a93df3f09debc4 |
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| 출처 메모 | uspto-grants-1988_05 |
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