Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → HCID 178453892, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 5-Fluoro-3-(4-piperidinyl)-1,2-benzisoxazole | HCID 2794755 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 반응물 | HCID 178453924 | HCID 178453924 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | HCID 178453892 | HCID 178453892 | 102% |
반응 단계
A mixture of 5-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (1.3 g, 5 mmol), trans-[4-(2-oxo-ethyl)-cyclohexyl]-carbamic acid tert-butyl ester (example 1, intermediate C) (1.6 g, 6 mmol), triethylamine (0.64 mL, 5 mmol) in 1,2 dichloroethane (27 mL) was stirred for 4 h at room temperature and sodium triacetoxyborohydride (1.9 g, 9 mmol) was added slowly and the resulting solution was stirred for 12 hours until the TLC indicated completion of the reaction. The mixture was filtrated and concentrated to dryness and purified with column chromatography on silica gel using CH2Cl2—CH2Cl2/MeOH (1-9:1). The product fractions were concentrated to give 2.3 g (5.1 mmol, 100% yield) of a off-white solid. MS (m/e): 446.3 (M+H+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08829029B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-376f96ff0f514fed88ddc6e5c17bd469 |
| 출처 메모 | uspto-grants-2014_09 |