참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4,4,5,8-Tetramethylthiochroman-6-carboxylic acid-1,1-dioxide | HCID 15869804 | — |
| 반응물 | Thiochroman carboxylic acid | HCID 19693770 | — |
| 반응물 | HCID 178418331 | HCID 178418331 | — |
| 반응물 | HCID 178418394 | HCID 178418394 | — |
| 용매 | 2-Methyl-2-butanol | HCID 6405 | — |
| 생성물 | HCID 178418286 | HCID 178418286 | 62.6% |
반응 단계
7.4 Grams (0.026 mol) of 4,4,5,8-tetramethylthiochroman-6-carboxylic acid-1,1-dioxide corresponding to thiochroman carboxylic acid (IIIc), 3.4 g (0.03 mol) of 1-ethyl-5-hydroxypyrazole corresponding to 5-hydroxypyrazole (II) and 6.22 g (0.03 mol) of DCC (N,N'-dicyclohexylcarbodiimide) were all together added to 50 ml of tert-amyl alcohol, and the mixture was stirred at room temperature for 30 minutes. Then, 1.8 g (0.013 mol) of anhydrous potassium carbonate was added. The reaction mixture was allowed to react at 80° C. for 8 hours, and the reaction solvent was distilled off under reduced pressure. The resultant residue was dispersed in a 5% potassium carbonate aqueous solution and ethyl acetate to separate it into two layers. Further, the aqueous layer was adjusted to a pH of 1 with 5% hydrochloric acid, and the formed solid was recovered by filtration to give 6.13 g (yield 62%) of 4,4,5,8-tetramethyl-6-(1-ethyl-5-hydroxypyrazol-4-yl)carbonylthiochroman-1,1-dioxide (Compound Ic-1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05723408 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
|---|
| ORD ID | ord-c66dc862259d4aac940736920bae0111 |
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| 출처 메모 | uspto-grants-1998_03 |
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