참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Chlorobenzyl mercaptan | HCID 80409 | — |
| 반응물 | 5-Iodo-2,3-dihydropyridazin-3-one | HCID 16638330 | — |
| 생성물 | 5-(4-chlorobenzylthio)pyridazin-3(2H)-one | HCID 58579857 | 51.9% |
반응 단계
A mixture of K2CO3 (65.4 mg, 0.47 mmol), (4-chlorophenyl)methanethiol (250 mg, 1.58 mmol), and 5-iodopyridazin-3(2H)-one (35 mg, 0.16 mmol) was stirred at 100° C. for 18 hours. After removal of the precipitate by filtration and concentration of the filtrate, the crude product was purified by prep-HPLC (C18 column/H2O:MeOH:TFA 90:10:0.1 to 10:90:0.1 gradient) to yield 5-(4-chlorobenzylthio)pyridazin-3(2H)-one 9A (21 mg, 51.6% yield). 1H NMR (400 MHz, Chloroform-D) δ ppm 11.08 (1H, br. s.), 7.57 (1H, d, J=2.01 Hz), 7.33 (4H, s), 6.57 (1H, d, J=2.01 Hz), 4.12 (2H, s).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08278316B2 |
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| 출처 데이터셋 | uspto-grants-2012_10 |
|---|
| ORD ID | ord-d648ca5a762e43f194855d28c73cd3e3 |
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| 출처 메모 | uspto-grants-2012_10 |
|---|
