참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diclofenac | HCID 3033 | — |
| 반응물 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 반응물 | Desmethylanethol trithione | HCID 3082127 | — |
| 반응물 | HCID 178418300 | HCID 178418300 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-Isothiocyanatophenyl 2-(2-(2,6-dichlorophenylamino)phenyl)acetate | HCID 25065770 | 23% |
반응 단계
To the solution of 1 (diclofenac, 1717 mg, 5.8 mmol) in 60 mL of dimethylformamide, hydroxybenzotriazole (862 mg, 6.38 mmol) and DCC (1316 mg, 6.38 mmol) were added with stirring at 0° C. for 1 h. To the reaction mixture 4-hydroxyphenylisothiocyanate (2; 965 mg, 6.38 mmol) was added and stirred for 1 h at 0° C. and 2 h at room temperature. After filtration, the filtrate was evaporated under reduced pressure to remove the solvent. The oily residue thus obtained was dissolved in ethyl acetate and the precipitate was removed. The solvent was evaporated and the crude product was loaded on a silica gel open column and eluted with chloroform/n-hexane 9:1, from which 4-isothiocyanatophenyl 2-(2-(2,6-dichlorophenylamino)phenyl)acetate (3) was obtained (580 mg, 23% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08541398B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-206a10ec26d64b0c904bc790354ed986 |
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| 출처 메모 | uspto-grants-2013_09 |
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