Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 5-(tert-Butyl-dimethyl-silanyloxy)-cyclooctanecarbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Tosylmethyl isocyanide | HCID 161915 | — |
| 반응물 | 5-(Tert-butyldimethylsilyloxy)cyclooctanone | HCID 10978090 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 5-(tert-Butyl-dimethyl-silanyloxy)-cyclooctanecarbonitrile | HCID 66656929 | — |
반응 단계
Potassium tert-butoxide (30.4 mL, 1 M in tetrahydrofuran, 30.4 mmol) was added drop wise to a stirred and cooled (0° C.) solution of tosylmethyl isocyanide (4.74 g, 24.27 mmol) in dry DME (40 mL). After ten minutes, dry methanol (0.98 mL, 24.28 mmol) was added and followed by a solution of the product of Example 5B (3.11 g, 12.14 mmol) in DME (10 mL). The resulting solution was allowed to warm to room temperature and then heated (45° C.) for thirty minutes. After cooling, the reaction mixture was partitioned with diethyl ether and water. The organic phase was washed with brine, dried (MgSO4), filtered, and evaporated. The residue was purified over silica gel using 2-10% diethyl ether in hexanes to give the title compound as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07737137B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-50778fe737ce4361906f6b8f685034de |
| 출처 메모 | uspto-grants-2010_06 |