Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Isoxazolecarbonyl chloride, 3-(2-chlorophenyl)-5-methyl- → 3-(2-Chlorophenyl)-5-methylisoxazole-4-carboxylic acid [4-dimethylamino-4-(3-fluorophenyl)cyclohexyl]amide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Isoxazolecarbonyl chloride, 3-(2-chlorophenyl)-5-methyl- | HCID 96590 | — |
| 반응물 | 1-(3-fluorophenyl)-N,N-dimethylcyclohexane-1,4-diamine | HCID 57904199 | — |
| 생성물 | 3-(2-Chlorophenyl)-5-methylisoxazole-4-carboxylic acid [4-dimethylamino-4-(3-fluorophenyl)cyclohexyl]amide | HCID 11698207 | — |
반응 단계
As described for Example 118, the polar diastereoisomer of 1-(3-fluorophenyl)-N,N-dimethylcyclohexane-1,4-diamine (350 mg) was reacted with 400 mg 3-(2-chlorophenyl)-5-methylisoxazole-4-carbonylchloride and worked up in a similar manner. The resultant crude product (590 mg) was chromatographed on silica gel (4.0×15 cm) with ethyl acetate/n-hexane/methanol (V:V=1:1:1). 440 mg of the polar diastereoisomer of 3-(2-chlorophenyl)-5-methylisoxazole-4-carboxylic acid [4-dimethylamino-4-(3-fluorophenyl)cyclohexyl]amide were obtained which, dissolved in 90 ml 2-butanone, were converted overnight into the corresponding hydrochloride by adding 17 μl water and 120 μl chlorotrimethylsilane (460 mg of white solid, Mp. 209-211° C.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08093272B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-14ca6306c8f748828ff64579126b26eb |
| 출처 메모 | uspto-grants-2012_01 |