참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | Tricyclohexylphosphine | HCID 75806 | — |
| 반응물 | 4-(Trifluoromethyl)phenylboronic acid | HCID 2734389 | — |
| 반응물 | 5-Iodo-2,3-dihydropyridazin-3-one | HCID 16638330 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 5-(4-(Trifluoromethyl)phenyl)pyridazin-3(2H)-one | HCID 57950387 | 39.1% |
반응 단계
Tricyclohexyl phosphine (16.6 μL, 0.02 mmol) was added to a mixture of 5-iodopyridazin-3(2H)-one (35 mg, 0.16 mmol), 4-(trifluoromethyl)phenylboronic acid (30 mg, 0.16 mmol), potassium phosphate tribasic (117 mg, 0.55 mmol), and palladium (II) acetate (3.5 mg, 0.02 mmol) in Toluene (0.8 mL) and Water (0.3 mL). The mixture was stirred at 100° C. for 22 hours. The reaction was diluted with CH2Cl2, filtered and concentrated. The crude was purified using HPLC (Phen Luna Axia C18 5μ 10:90:0.1 to 90:10:0.1 MeOH—H2O-TFA) to afford the desired product 5-(4-(trifluoromethyl)phenyl)pyridazin-3(2H)-one 18A (14.8 mg, 0.06 mmol, 39.1% yield) as a white solid. LC/MS 282 (M+H)+, tR 0.77 min (method 5).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08278316B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_10 |
|---|
| ORD ID | ord-298cfe593174440d8b9f2ab3d35484b9 |
|---|
| 출처 메모 | uspto-grants-2012_10 |
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