Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tributylphosphine → Methyl(4-chloro-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tributylphosphine | HCID 13831 | — |
| 반응물 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 반응물 | (2-Methyl-6-(trifluoromethyl)pyridin-3-yl)methanol | HCID 2760122 | — |
| 반응물 | Methyl(4-chloro-6-hydroxy-1-benzothiophen-3-yl)acetate | HCID 20770824 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Methyl(4-chloro-6-((2-methyl-6-(trifluoromethyl)pyridin-3-yl)methoxy)-1-benzothiophen-3-yl)acetate | HCID 71721632 | 89% |
반응 단계
To a mixture of methyl(4-chloro-6-hydroxy-1-benzothiophen-3-yl)acetate (110 mg) and THF (dry) (5 mL) were added (2-methyl-6-(trifluoromethyl)pyridin-3-yl)methanol (82 mg), tri-n-butylphosphine (0.159 mL), and ADDP (130 mg) at room temperature. The mixture was stirred at room temperature for 12 h. The insoluble material was removed by filtration, and the filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (164 mg). The compound was crystallized from IPE-hexane.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09238639B2 |
| 출처 데이터셋 | uspto-grants-2016_01 |
| ORD ID | ord-c692b59b4e41434f8b4cde10088f6389 |
| 출처 메모 | uspto-grants-2016_01 |