참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | tert-Butyl methyl ether | HCID 15413 | — |
| 반응물 | Sodium Sulfite | HCID 24437 | — |
| 반응물 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 반응물 | 4-Chloro-5-(cyclopropylmethoxy)-2-methylsulfanylpyrimidine | HCID 118024111 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Chloro-5-(cyclopropylmethoxy)-2-methylsulfonylpyrimidine | HCID 118022445 | 78.3% |
반응 단계
To the title compound of step 3 (19.0 g, 82.60 mmol) in dry CH2Cl2 (200 mL) at 0° C., m-CPBA (42.62 g, 247.80 mmol) was added over 15 min. The mixture was stirred at 0° C. for 30 min and at r.t. overnight. Sat.aq. Na2SO3 (100 mL) was added and CH2Cl2 extractive work up was carried out. Trituration with MTBE (300 mL) gave the title compound (17 g, 78.3% yield) as a white solid. 1H NMR (CDCl3, 400 MHz) δ 8.37 (s, 1H), 4.13 (d, J=6.8 Hz, 2H), 3.33 (s, 3H), 1.39-1.35 (m, 1H), 0.79-0.74 (m, 2H), 0.49-0.45 (m, 2H). LCMS: 263.0 (M+1)+
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09034900B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_05 |
|---|
| ORD ID | ord-f73e5778be1944469d0a00d81ba25250 |
|---|
| 출처 메모 | uspto-grants-2015_05 |
|---|