참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Boron trifluoride etherate | HCID 8000 | — |
| 반응물 | 7-Aminocephalosporanic acid | HCID 441328 | — |
| 반응물 | HCID 178482016 | HCID 178482016 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178482015 | HCID 178482015 | 80% |
반응 단계
A solution of 1.54 g. of 7-aminocephalosporanic acid and 1.0 g. (5 mmole) of 1-(1-methyl-1H-tetrazol-5-ylmethyl)-1H-tetrazol-5-thiol in 7.0 ml. of glacial acetic acid was heated in an oil bath to a temperature of about 65°-70° C. To the hot reaction mixture were added 3.6 ml. of boron trifluoride etherate, and the reaction mixture was heated at a temperature of 65°-70° C. for one hour with stirring. The reaction mixture was then cooled to room temperature and 10 ml. of water were added. The reaction mixture was stirred for 15 minutes after water addition, was filtered, and then chilled in an ice bath. The pH of the cold mixture was adjusted to pH 4.5 with concentrated ammonium hydroxide. The precipitate which formed was filtered, washed repeatedly with water, with acetone, and finally with diethyl ether. The off-white solid product was vacuum dried for one hour at 40° C. There was obtained 1.5 g. (80% yield) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04346076 |
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| 출처 데이터셋 | uspto-grants-1982_08 |
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| ORD ID | ord-c828cb921753496e9f48c31b62f15f2f |
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| 출처 메모 | uspto-grants-1982_08 |
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