Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tributylphosphine → {4-[3-Bromo-5-(3-morpholin-4-yl-propoxy)-phenylsulfanyl]-2-chloro-phenoxy}-acetic Acid Ethyl Ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tributylphosphine | HCID 13831 | — |
| 반응물 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 반응물 | 3-Morpholino-1-propanol | HCID 199576 | — |
| 반응물 | [4-(3-Bromo-5-hydroxy-phenylsulfanyl)-2-chloro-phenoxy]-acetic Acid Ethyl Acetate | HCID 67024266 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | {4-[3-Bromo-5-(3-morpholin-4-yl-propoxy)-phenylsulfanyl]-2-chloro-phenoxy}-acetic Acid Ethyl Ester | HCID 57791920 | — |
반응 단계
[4-(3-Bromo-5-hydroxy-phenylsulfanyl)-2-chloro-phenoxy]-acetic acid ethyl acetate (1.7 g; 4.07 mmol), N-(3-hydroxypropyl)morpholine (0.59 g; 4.07 mmol) and tributylphosphine (1.8 g; 7.33 mmol) were dissolved in THF (100 mL) in a dried reaction flask under an atmosphere of nitrogen. 1,1′-(Azodicarbonyl)dipiperidine (1.85 g; 7.33 mmol) dissolved in THF (50 mL) was added to the reaction mixture, which was stirred at room temperature for 16 h. The reaction mixture was evaporated to dryness and purified by flash chromatography (ethyl acetate:heptane). Yield: 1.1 g. HPLC-MS: m/z: 544.0 (M+); Rt: 1.78 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07943669B2 |
| 출처 데이터셋 | uspto-grants-2011_05 |
| ORD ID | ord-ae040c11c28b47dcb2c53d3addc235f1 |
| 출처 메모 | uspto-grants-2011_05 |