참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | 4,6-Dichloro-5-fluoro-2-(methylsulfanyl)pyrimidine | HCID 22378277 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-Chloro-5-fluoro-6-hydrazino-2-(methylthio)pyrimidine | HCID 86636914 | 59% |
반응 단계
4,6-Dichloro-5-fluoro-2-(methylthio)pyrimidine (16.8 g, 78.85 mmol) and triethylamine (16.49 mL, 118.3 mmol) were dissolved in DMSO (200 mL) and stirred. The mixture was cooled to ˜5° C. with an ice water bath. To this solution was slowly added hydrazine monohydrate (4.59 mL, 94.62 mmol). After the addition was complete, the reaction mixture was warmed up to RT and stirring was continued for 1 h. The reaction mixture was diluted with water (500 mL), and the aqueous solution was extracted with CH2Cl2 (3×300 mL). The combined organic solution was washed with water (3×250 mL) and brine (250 mL), then dried (Na2SO4) and concentrated in vacuo to afford 4-chloro-5-fluoro-6-hydrazino-2-(methylthio)pyrimidine as a red foamy solid (9.70 g, 59%). LCMS: (M+H)+: 208.9.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07893056B2 |
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| 출처 데이터셋 | uspto-grants-2011_02 |
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| ORD ID | ord-ac801d8532914b6f9d5ae02facebb00e |
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| 출처 메모 | uspto-grants-2011_02 |
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