참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Fluoro-2-nitrobenzene | HCID 73895 | — |
| 반응물 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 반응물 | 2-Amino-5-methylbenzonitrile | HCID 242778 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 5-Methyl-2-(2-nitro-phenylamino)-benzonitrile | HCID 21093537 | 57.1% |
반응 단계
Combine 1-fluoro-2-nitro-benzene (4.34 g, 30.79 mmol), 2-amino-5-methyl-benzonitrile (4.07 g, 30.79 mmol), lithium hydroxide monohydrate (2.58 g, 61.58 mmol) and DMSO (50.0 ml). Stir the mixture at 55° C. for 22 hours then cool it to ambient temperature. Pour the mixture onto ice chips and stir for 1 hour. Remove the resulting precipitate by vacuum filtration. Dry the precipitate under vacuum then purify it on silica gel using dichloromethane/hexanes (75:25) to give 4.45 g (57%) of an orange solid: mp 135–139°; mass spectrum (ion spray): m/z=254.0 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07214673B2 |
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| 출처 데이터셋 | uspto-grants-2007_05 |
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| ORD ID | ord-d3511f8fa69d4768965c2c5393b39b32 |
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| 출처 메모 | uspto-grants-2007_05 |
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