참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | Sodium Sulfite | HCID 24437 | — |
| 반응물 | 1H-Pyrazole, 3-methyl-5-(trifluoromethyl)- | HCID 139077 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-Bromo-3-methyl-5-(trifluoromethyl)pyrazole | HCID 2736430 | 100% |
반응 단계
Dissolve 5-methyl-3-(trifluoromethyl)pyrazole (1.00 g, 6.66 mmol) in 60% aqueous acetic acid (13 mL). Add sodium acetate (0.819 g, 9.99 mmol) and cool to 0° C. Add bromine (1.17 g, 7.33 mmol) dropwise over 10 min. Stir at 0° C. for 3 hr, then at room temperature for 18 hr. Add ethyl acetate and saturated aqueous sodium sulfite solution. Separate organics and wash one time with saturated aqueous sodium bicarbonate solution followed by saturated aqueous sodium chloride. Dry (magnesium sulfate), filter and concentrate to give 4-bromo-5-methyl-3-trifluoromethyl-1H-pyrazole (1.50 g, 100%). GC-MS: m/z=229 [M+].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08202873B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_06 |
|---|
| ORD ID | ord-33e599f9ee714cb982e2ab2c1ef6a0fd |
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| 출처 메모 | uspto-grants-2012_06 |
|---|
