참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dabco | HCID 9237 | — |
| 반응물 | Pivalaldehyde | HCID 12417 | — |
| 반응물 | 3-Aminopyrrolidine | HCID 164401 | — |
| 반응물 | 3-(2,2-Dimethylpropylideneamino)-pyrrolidine | HCID 14836604 | — |
| 반응물 | 8-Chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-3-quinolinecarboxylic acid | HCID 19694999 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Clinafloxacin | HCID 60063 | — |
반응 단계
0.95 g (11 mmol) of pivalaldehyde are added dropwise to a solution of 0.86 g (10 mmol) of 3-aminopyrrolidine in 10 ml of acetonitrile at room temperature in the course of 5 minutes, during which the temperature rises from 22.5° C. to 27.5° C. The mixture is subsequently stirred for 1 hour and a virtually complete conversion into 3-(2,2-dimethylpropylideneamino)-pyrrolidine is found by checking the reaction by gas chromatography. The mixture is then diluted with 10 ml of acetonitrile and 10 ml of dimethylformamide, 3 g (10 mmol) of 8-chloro-1-cyclopropyl-6,7-difluoro-1,4-dihydro-3-quinolinecarboxylic acid and 2.2 g (20 mmol) of 1,4-diazabicyclo[2.2.2]octane are added and the mixture is heated under reflux for 1 hour. Work up gives the same result as described under Example 2a).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05723627 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
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| ORD ID | ord-182cab8e991e46b5ad9d638c603333a5 |
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| 출처 메모 | uspto-grants-1998_03 |
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