참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ethyl bromoacetate | HCID 7748 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 6-fluoro-5-nitro-2(3H)-benzothiazolone | HCID 13957955 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-ethoxycarbonylmethyl-6-fluoro-5-nitro-2(3H)-benzothiazolone | HCID 14014244 | 25% |
반응 단계
50% Oily sodium hydride (0.21 g) was suspended in N,N-dimethylformamide (5 ml), and the resultant suspension was cooled to 0° C. 6-Fluoro-5-nitro-2(3H)-benzothiazolone (1.0 g) was portionwise added thereto at 0° C., and the mixture was stirred at the same temperature for 30 minutes. Ethyl bromoacetate (0.86 g) was added to the reaction mixture at 0° C., and the temperature was gradually elevated to a temperature of 50° to 60° C., followed by stirring at that temperature for 3 hours. Water was added to the mixture, which was extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The residue was purified by silica gel thin layer chromatography with a mixture of ethyl acetate and toluene (1:9) to give 0.35 g of 3-ethoxycarbonylmethyl-6-fluoro-5-nitro-2(3H)-benzothiazolone, m.p., 139.0°-140.0° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04888428 |
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| 출처 데이터셋 | uspto-grants-1989_12 |
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| ORD ID | ord-33779e788a05417badbe4024f628ef3d |
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| 출처 메모 | uspto-grants-1989_12 |
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