참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-Propanol, 1-amino-2-methyl- | HCID 95102 | — |
| 반응물 | 5-Fluoro-2-nitroanisole | HCID 2779250 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-(3-Methoxy-4-nitrophenylamino)-2-methylpropan-2-ol | HCID 65109358 | — |
반응 단계
A 20 mL reaction vial equipped with a stir bar was charged with 4-fluoro-2-methoxy-1-nitrobenzene (0.5 g, 2.92 mmol), 1-amino-2-methylpropan-2-ol (0.313 g, 3.51 mmol), N-methyl-2-pyrrolidinone (7.3 mL) and Hunig's base (N,N-diisopropylethylamine) (0.76 g, 5.84 mmol). The vessel was sealed and the reaction was heated on a thermal block at 80° C. for 24 hours. The reaction was cooled to ambient temperature, treated with water (40 mL) and extracted with ethyl acetate (3×60 mL). The combined organic layers were washed with brine (25 mL), dried over Na2SO4, filtered, and concentrated. The concentrate was purified by flash chromatography on a 10 g silica gel column with 1% methanol/CH2Cl2 to provide the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08536180B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-c98108077fe4464e8dc39edb59beb0a9 |
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| 출처 메모 | uspto-grants-2013_09 |
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