Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dicyclohexylcarbodiimide → HCID 53971898, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 1-Chloro-5-fluoro-4-isothiocyanato-2-[(propan-2-yl)oxy]benzene | HCID 13607933 | — |
| 반응물 | 4-Fluoro-L-proline | HCID 22214888 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 53971898 | HCID 53971898 | 89.8% |
반응 단계
A mixture of 1.31 g (0.01 mol) 4-fluoroproline, 30 mL 2N KOH in methanol and 10 mL water is prepared before 2.46 g (0.01 mol) 4-chloro-2-fluoro-5-isopropoxy-phenylisothiocyanate dissolved in 250 mL methanol is added dropwise. The reaction mixture is stirred overnight at room temperature, the aqueous phase adjusted to pH 2 and the resultant product (3.77 g, See Formula X) is filtered. The compound thus obtained is dissolved in 50 mL acetonitrile before 2.59 g (0.01 mol) dicyclohexylcarbodiimide is added at room temperature. The reaction mixture is stirred for 3 h and the crude product is purified by silica gel chromatography to give 3.24 g (85% yield) of the desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05712225 |
| 출처 데이터셋 | uspto-grants-1998_01 |
| ORD ID | ord-804654d342e24569ad4a9a350c28f6c9 |
| 출처 메모 | uspto-grants-1998_01 |