참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 2-Thiophenecarbothioamide | HCID 737237 | — |
| 반응물 | HCID 86756575 | HCID 86756575 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | HCID 22009660 | HCID 22009660 | 63% |
반응 단계
Acetic acid (3.78 ml) was added to a stirred mixture of 2-thiophenecarbothioamide (3.15 g), ethyl chloroformylacetate potassium salt (6.23 g) and ethanol (60 ml). Afte refluxing for 4 h, ethyl chloroformylacetate potassium salt (4.15 g) and acetic acid (2.52 ml) were added, and then the refluxing was continued for further 20 h. The reaction mixture was concentrated, diluted with saturated aqueous sodium bicarbonate, and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and concentrated to give an oil which was purified by silica gel column chromatography. From the fraction eluted with ethyl acetate-hexane (1:1, v/v) the crystals of ethyl 2-(2-thienyl)-5-thiazolecarboxylate (3.29 g, 63%) were obtained. Recrystallization from ethyl acetate-hexane gave colorless needles, mp 61-62° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06211215B1 |
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| 출처 데이터셋 | uspto-grants-2001_04 |
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| ORD ID | ord-1cdddae9b597462c85738ff34a12fc05 |
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| 출처 메모 | uspto-grants-2001_04 |
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