참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 2,6-Dimethylphenol | HCID 11335 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1,2-Benzenedicarbonitrile, 4-nitro- | HCID 97443 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-(2',6'-Dimethylphenoxy)phthalonitrile | HCID 952073 | 87% |
반응 단계
A mixture of 4-nitro-phthalonitrile (1 eq), 2,6-dimethylphenol (1.2 eq), K2CO3 (2 eq), and DMF (1 mL/mmol 4-nitro-phthalonitrile) was heated under nitrogen at 60° C. for 3 h with stirring. After cooling to ambient temperature the mixture was poured into water (6 mL/mL DMF) with stirring. The mixture was extracted twice with EtOAc. The combined organic phases were dried over MgSO4 and concentrated in vacuo. The residue was recrystallized from EtOH to give the title compound as a tan solid (yield: 87%); 1H NMR (CDCl3, 200 MHz): δ=7.70 (d, 1H), 7.05 to 7.16 (m, 5H), 2.08 (s, 6H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09174976B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-3eaf6c55f8e84abc82d5bd711741b9d7 |
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| 출처 메모 | uspto-grants-2015_11 |
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