참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,4-Dichlorophthalazine | HCID 78490 | — |
| 반응물 | 7-Methoxy-2-naphthol | HCID 853173 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | 1-(4-Chlorophthalazin-1-yl)-7-methoxynaphthalen-2-ol | HCID 136343453 | 80% |
반응 단계
In a 1 L flask under nitrogen were mixed 1,4-dichlorophthalazine (11.4 g, 57.3 mmol) with 7-methoxy-naphthalen-2-ol (10.0 g, 57.5 mmol). To this was added 1,2-dichloroethane (450 ml). After stirring for 10 min, aluminum chloride (7.64 g, 57.4 mmol) was added. The resulting suspension was stirred for 20 hrs at 80° C. After cooling to room temperature, the black suspension was poured on ice-water (500 ml) and stirred for 1 hr. The two layers were separated. The aqueous layer was extracted with dichloromethane (3×200 ml). The combined organic layers were dried over sodium sulfate and concentrated under reduced pressure. The crude solid was triturated with dichloromethane (35 ml) for 1 hr and collected by filtration to give 15.2 g of the title compound as a grey solid. (Yield: 80%)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07790882B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_09 |
|---|
| ORD ID | ord-ed23b821dc2e4ab4985a78b5a2f88016 |
|---|
| 출처 메모 | uspto-grants-2010_09 |
|---|