참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Persulfate | HCID 24412 | — |
| 반응물 | Potassium bisulfate | HCID 516920 | — |
| 반응물 | 2-(Methylsulfanyl)pyrimidine | HCID 522772 | — |
| 반응물 | Potassium hydroxy sulfite | HCID 23707502 | — |
| 반응물 | 6-Cyclopropyl-2-(methylsulfanyl)pyrimidine-4-carboxylic acid | HCID 39870841 | — |
| 반응물 | 6-Cyclopropyl-2-(methylsulfonyl)pyrimidine-4-carboxylic acid | HCID 67983412 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Methyl 6-cyclopropyl-2-(methylsulfonyl)pyrimidine-4-carboxylate | HCID 67983976 | — |
반응 단계
6-cyclopropyl-2-(methylsulfonyl)pyrimidine-4-carboxylic acid (I-20A). Into a 40 mL vessel was added 6-cyclopropyl-2-(methylthio)pyrimidine-4-carboxylic acid_(commerically available, Enamine Ltd, catalog number EN300-422464, 250 mg, 1.19 mmol) and acetonitrile (12.5 mL). This resulting solution was then added dropwise at RT over 5 min. to a separate 40 mL reaction vessel that was charged with a rapidly stirred suspension of Oxone™ (using Aldrich supplied Oxone which is a multicomponent triple salt mixture containing potassium monopersulfate, 2 KHSOs5.KHSO4.K2SO4, 2.50 g, 4.10 mmol) and water (15 mL). Upon complete addition of the methyl thiopyrimidine, the resulting suspension was heated to 65° C. for 20 min. and subsequently cooled to RT. The resulting yellow suspension was extracted with ethyl acetate (4×100 mL) and the organic extracts were dried over magnesium sulfate, filtered and concentrated to furnish the methyl sulfonyl pyrimidine as a residue that was used directly in the next step without isolation. MS m/z 243.1 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09150568B2 |
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| 출처 데이터셋 | uspto-grants-2015_10 |
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| ORD ID | ord-fa3dd2f3bcc74a7c85557b224e553005 |
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| 출처 메모 | uspto-grants-2015_10 |
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