참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylbarbituric acid | HCID 69860 | — |
| 반응물 | 1-[2-(4-Allyloxy-phenylmethanesulfinyl)-ethyl]-1H-[1,2,3]triazole | HCID 22242085 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-(2-[1,2,3]Triazol-1-yl-ethanesulfinylmethyl)-phenol | HCID 22242075 | 97.5% |
반응 단계
A solution of 1.00 g (3.43 mmol) 1-[2-(4-allyloxy-phenylmethanesulfinyl)-ethyl]-1H-[1,2,3]triazole in 60 ml dichloromethane was added to a solution of 1.61 g (10.3 mmol) 1,3-dimethylbarbituric acid and 102 mg (0.09 mmol) Pd(PPh3)4 in 30 ml dichloromethane and stirred for 5 h at 50° C. The mixture was extracted with 3×50 ml sat. NaHCO3-solution and 20 ml water. The organic phase was discarded and the aqueous phase acidified with 2M HCl to pH=4, concentrated to a volume of 50 ml and adjusted to pH=1. After five extractions with ethyl acetate, the organic extracts were combined and dried over MgSO4. After evaporation the residue was purified by chromatography on silica gel (dichloromethane/methanol 100:2) to yield 0.84 g (97%) of 4-(2-[1,2,3]Triazol-1-yl-ethanesulfinylmethyl)-phenol.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07429605B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-d9c2db7229934015a6ccd109b303a010 |
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| 출처 메모 | uspto-grants-2008_09 |
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