Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,6-Dichloro-3-methylaniline → 8-(cyclopentyloxy)-4-(2,6-dichloro-3-methylphenylamino)-7-methoxy-2H-chromen-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,6-Dichloro-3-methylaniline | HCID 116529 | — |
| 반응물 | Monobasic potassium phosphate | HCID 516951 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 반응물 | 4-chloro-8-(cyclopentyloxy)-7-methoxy-2H-chromen-2-one | HCID 77174794 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 8-(cyclopentyloxy)-4-(2,6-dichloro-3-methylphenylamino)-7-methoxy-2H-chromen-2-one | HCID 24849477 | — |
반응 단계
Potassium t-butoxide (35 mg, 0.3 mmol) was added to a solution of 4-chloro-8-(cyclopentyloxy)-7-methoxy-2H-chromen-2-one (29 mg, 0.1 mmol, Example 7, Step 1), 2,6-dichloro-3-methylaniline (26 mg, 0.15 mmol), and DMSO (1 mL). After 14 h, the reaction was poured into 1M KH2PO4 (20 mL), and extracted with ethyl acetate (20 mL×2). The combined extracts were dried, filtered, concentrated, and purified by silica gel chromatography (4:1→0:1; hexanes:ethyl acetate) to give 8-(cyclopentyloxy)-4-(2,6-dichloro-3-methylphenylamino)-7-methoxy-2H-chromen-2-one: 1H NMR (400 MHz, DMSO-d6): δ 9.38 (s, 1H), 7.95 (d, 1H), 7.58 (d, 1H), 7.48 (d, 1H), 7.18 (d, 1H), 4.82 (m, 1H), 4.33 (s, 1H), 3.90 (s, 3H), 2.40 (s, 3H), 1.90-1.45 (m, 8H); MS (ESI): 433.9.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07745646B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-25a63d98a37b4e3c9603f7eb11e4e24c |
| 출처 메모 | uspto-grants-2010_06 |