참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Ethyl 1,2,3-thiadiazole-4-carboxylate | HCID 254337 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | Ethyl 1,2,3-thiadiazole-4-carboxylate | HCID 254337 | 7% |
| 생성물 | 1,2,3-Thiadiazol-4-ylmethanol | HCID 14727409 | 18% |
반응 단계
To a suspension of ethyl 1,2,3-thiadiazol-4-ylcarboxylate (18.35 g, 0.116 mol) in ether (400 mL) was added portionwise lithium aluminum hydride (2.47 g, 0.065 mol) over 1 h period. The reaction mixture was stirred at 23° C. for 7 h and treated with lithium aluminum hydride (2.47 g, 0.065 mL). The stirring was continued for 24 h before adding successively water (7 mL), 15% sodium hydroxide solution (7 mL) and water (21 mL). After stirring for 15 min, the ether solution was decanted and the gum was extracted with ether (5×100 mL). The ether extracts were combined, dried (MgSO4) and concentrated (5.4 g). The crude material was purified on silica gel column (120 g, 4×16 cm), with ether as eluting solvent to give 1.3 g (7%) of ethyl 1,2,3-thiadiazol-4-ylcarboxylate and 2.45 g (18%) of 1,2,3-thiadiazol-4 -ylmethanol;
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04746736 |
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| 출처 데이터셋 | uspto-grants-1988_05 |
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| ORD ID | ord-218feb220ed0459b954fe03cb3f3880f |
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| 출처 메모 | uspto-grants-1988_05 |
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