참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | Ditert-butyl 1-chlorocyclopropane-1,2-dicarboxylate | HCID 23158970 | — |
| 촉매 | Dichlorocobalt hexahydrate | HCID 517166 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | Di-tert-butyl cyclopropane-1,2-dicarboxylate | HCID 23158971 | 96% |
반응 단계
Sodium borohydride (103 mg, 1.81 mmol) was added to and dissolved in N,N-dimethylacetamide (1.5 mL) at room temperature, followed by addition of an N,N-dimethylacetamide solution (1.0 mL) of di-tert-butyl 1-chlorocyclopropane-1,2-dicarboxylate (cis/trans=26/74) (hereinafter the compound will be referred to as “compound (4b)”) (500 mg, 1.81 mmol) at 10° C. Cobalt chloride hexahydrate (2.4 mg, 0.010 mmol) was added to the resultant solution at the same temperature. After completion of addition, the resultant mixture was stirred at 40° C. for six hours. After completion of reaction, the whole reaction mixture was diluted with an HPLC mobile phase to 50 mL, to thereby yield a solution containing 418.8 mg (yield: 96%) of the title compound. Yield was determined by means of high performance liquid chromatography (HPLC) (the same shall apply hereinafter).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07381833B2 |
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| 출처 데이터셋 | uspto-grants-2008_06 |
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| ORD ID | ord-a200717bb849434e8ad323295c482c61 |
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| 출처 메모 | uspto-grants-2008_06 |
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