Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl pivaloylacetate → 3,3-Dimethyl-1-[3-(3-nitrophenyl)-1,2,4-oxadiazol-5-yl]butan-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl pivaloylacetate | HCID 99597 | — |
| 반응물 | N'-hydroxy-3-nitrobenzenecarboximidamide | HCID 3781554 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3,3-Dimethyl-1-[3-(3-nitrophenyl)-1,2,4-oxadiazol-5-yl]butan-2-one | HCID 16655132 | 90% |
반응 단계
In a 250 ml flask, place 16 g (0.088 m) of 3-nitrobenzamidoxime (9a), 21.3 g (0.135 m) of methyl 4,4-dimethyl-3-oxovalerate (10a; R1=t-butyl), and 120 ml of toluene. Heat and stir the reaction mixture under reflux with a Dean-Stark trap for 23 hrs. Distill off toluene under a reduced pressure at 50-60° C. to thick oil. Add 60 ml of heptane to the oil with stirring, cool and stir at 0-5° C. for 30 min. Collect solid, wash with heptane, and dry in air to give 22.9 g (90%) of 5-(3,3-dimethyl-2-oxobutyl)-3-(3-nitrophenyl)-1,2,4-oxadiazole [Formula I: R1=t-butyl and R2=3-nitrophenyl].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07312337B2 |
| 출처 데이터셋 | uspto-grants-2007_12 |
| ORD ID | ord-73330b78bb334b04b3d58213c4513782 |
| 출처 메모 | uspto-grants-2007_12 |