Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 4-{[3-(Trimethoxysilyl)propyl]thio}-4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-2-butanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | (3-Mercaptopropyl)trimethoxysilane | HCID 20473 | — |
| 반응물 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 반응물 | Alpha-Ionone | HCID 5282108 | — |
| 생성물 | 4-{[3-(Trimethoxysilyl)propyl]thio}-4-(2,6,6-trimethyl-2-cyclohexen-1-yl)-2-butanone | HCID 68815435 | 71.3% |
반응 단계
To a stirred solution of α-ionone (1.92 g, 10.0 mmol) and 3-mercaptopropyl-trimethoxysilane (1.96 g, 10.0 mmol) at 12° C. was rapidly added DBU (0.14 ml, 152 mg, 1.0 mmol). The temperature rose to 19° C. and the solution turned orange. After 135 minutes at 20° C, the reaction mixture was poured onto a cold stirred 5% aqueous HCl solution and extracted twice with Et2O. The organic phases were washed (H2O, saturated aqueous NaHCO3 and brine), dried (Na2SO4), filtered and concentrated. The crude extract was dried for 1 hour at 65-70° C./0.01 Torr to give 2.77 g of the title thioether (71%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07589055B2 |
| 출처 데이터셋 | uspto-grants-2009_09 |
| ORD ID | ord-c9d5ac5521e349c7a2a62136574918c6 |
| 출처 메모 | uspto-grants-2009_09 |