Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 4-(1-(N-acetyl-N-methylamino)cyclopropyl)anisole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-(1-(N-Acetylamino)cyclopropyl)anisole | HCID 19066431 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ammonium Chloride | HCID 25517 | — |
| 생성물 | 4-(1-(N-acetyl-N-methylamino)cyclopropyl)anisole | HCID 19066497 | 73.4% |
반응 단계
To a stirred suspension of 60% sodium hydride (234 mg, 5.85 mmol) (washed with pentane) in dry DMF (20 ml) was added Compound 8 (1.00 g, 4.87 mmol) portionwise at room temperature. After 15 min., to this was added iodomethane (1.04 g, 7.31 mmol) at same temperature. The reaction mixture was stirred at room temperature for 2 h. The mixture was diluted with sat. NH4Cl aq. (20 ml)-H2O (20 ml) and extracted with toluene-AcOEt (1:2). The combined solution was washed with water and brine, dried(MgSO4) and concentrated in vacuo to give crude product (1.05 g) as a yellow solid. The crude product was recrystallized from hexane-ethyl acetate to give Compound 9 (784 mg, 73%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05789423 |
| 출처 데이터셋 | uspto-grants-1998_08 |
| ORD ID | ord-93e42b44c33b4d50a7f666f8061788fc |
| 출처 메모 | uspto-grants-1998_08 |