Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Iodide → 4-[3-(3-Butylidene-8-aza-bicyclo[3.2.1]oct-8-yl)-propyl]-4H-benzo[1,4]oxazin-3-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-(3-chloropropyl)-2H-1,4-benzoxazin-3(4H)-one | HCID 23345150 | — |
| 반응물 | 3-Butylidene-8-azabicyclo[3.2.1]octane | HCID 68911083 | — |
| 용매 | Dichloromethane methanol | HCID 21226129 | — |
| 생성물 | 4-[3-(3-Butylidene-8-aza-bicyclo[3.2.1]oct-8-yl)-propyl]-4H-benzo[1,4]oxazin-3-one | HCID 68908216 | 41.2% |
반응 단계
4-(3-Chloropropyl)-4H-benzo[1,4]oxazin-3-one (81MF08) (0.030 g, 0.13 mmol), K2CO3 (0.037 g, 0.26 mmol), NaI (0.040 g, 0.27 mmol) and 3-butylidene-8-azabicyclo[3.2.1]octane (0.029 g, 0.17 mmol) were mixed according to GP12. Prep TLC (SiO2; CH2Cl2/MeOH 10:1) gave the title compound (81MF24) (0.019 g, 41%). 1H NMR (CDCl3) δ7.22-7.19 (m, 1H), 7.05-6.96 (m, 3H), 5.24 (t, J=7.2 Hz, 1H), 5.08 (s, 2H), 4.06 (t, J=6.4 Hz, 2H), 2.61 (t, J=6.8 Hz, 2H), 2.30 (s, 2H), 2.03-1.83 (M, 7H), 1.58-1.43 (m, 2H), 1.39-1.22 (m, 3 H), 0.89 (m, 3 H); 13C NMR (CDCl3) δ164.5, 145.5, 128.7, 127.9, 124.0, 123.0, 117.1, 115.5, 67.8, 60.4, 60.2, 48.8, 41.0, 39.6, 33.7, 29.5, 26.8, 26.4, 25.8, 23.2, 13.9.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07307075B2 |
| 출처 데이터셋 | uspto-grants-2007_12 |
| ORD ID | ord-1dd19d7ce52a45f3a93f9226cdcf7b97 |
| 출처 메모 | uspto-grants-2007_12 |