Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetonitrile → 8-(4-(Methylsulfonyl)phenyl)-1,4-dioxa-8-azaspiro[4.5]decane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| 반응물 | 1-Fluoro-4-(methylsulphonyl)benzene | HCID 67994 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 8-(4-(Methylsulfonyl)phenyl)-1,4-dioxa-8-azaspiro[4.5]decane | HCID 4256360 | 77.3% |
반응 단계
A mixture of 10 g (0.057 mol) of p-fluorophenyl methyl sulfone, 8.72 g (0.063 mol) of K2CO3, 24.66 g (0.172 mol) of 1,4-dioxa-8-azaspiro[4.5]-decane and 50 ml of acetonitrile is stirred overnight at 90°-100° C. After cooling, the mixture is diluted with water and extracted with methylene chloride. The combined extracts are washed with brine, dried over Na2SO4, and concentrated in vacuo. Trituration with ethyl ether affords 13.11 g (77%) of title compound as a white solid: m.p. 192°-194° C.; IR (KBr) 1588, 1369, and 1290 cm-1 ; NMR (CDCl3) δ 7.74 (m, 2H), 6.96 (m, 2H), 4.02 (s, 4H), 3.54 (m, 4H), 3.03 (s, 3H), and 1.81 (m, 4H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04894374 |
| 출처 데이터셋 | uspto-grants-1990_01 |
| ORD ID | ord-7a0af4ea29a74a42902eadeffd979f2f |
| 출처 메모 | uspto-grants-1990_01 |