참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Benzoic acid, 2-amino-6-fluoro-3-nitro-, ethyl ester | HCID 2756434 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Amino-3-nitro-6-(2,2,2-trifluoro-ethoxy)-benzoic acid ethyl ester | HCID 68616107 | — |
반응 단계
420 mg NaH (60% suspension in oil) were added to a solution of 2.16 mL (29.8 mmol) 2,2,2-trifluoro-ethanol in 5 mL THF. When the gas evolution ceased, 1.0 g (4.38 mmol) 2-Amino-6-fluoro-3-nitro-benzoic acid ethyl ester was added. The resulting mixture was stirred at 0° C. for 30 minutes and at room temperature for further 30 minutes. To this mixture were added 2 mL of a 6 M aqueous HCl-solution, and most of the solvent was removed under reduced pressure. The residue was mixed with 20 mL water and the resulting solid was collected and washed with water and then hexane. The obtained yellow crystalline material was dried under reduced pressure at 35° C. Yield: 1.22 g.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07741341B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-72e6377cac6543abae76d361f020c377 |
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| 출처 메모 | uspto-grants-2010_06 |
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