참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Tributylstannane | HCID 5948 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | HCID 14281586 | HCID 14281586 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 용매 | Acetonitrile ether | HCID 21885917 | — |
| 생성물 | HCID 14854210 | HCID 14854210 | 90% |
반응 단계
To 700 mg (1.657 mMol) of 4-t-butyl 7β-t-butyloxycarbonylamino-3-allyloxycarbonyl-1-carba-3-cephem-4-carboxylate, dissolved in 12 ml of (1:1) CH3CN/(CH3CH2)2O, was added 174 mg (0.663 mMol) of triphenylphosphine and 20.34 mg (0.0829 mMol) of ##STR153## The reaction mixture was stirred for approximately 20 minutes and then cooled to 0° C. and treated with 0.464 ml (1.724 l) of (CH3CH2CH2CH2)3SnH. The reaction mixture was then allowed to cool and stirring was continued for 50 minutes. The crude reaction mixture was then treated with 1N HCl. This mixture was then poured into 100 ml of CHCl3 and 25 ml of H2O. The organic layer was separated, dried over anhydrous MgSO4, filtered, and concentrated, under reduced pressure to provide an oily solid. The crude product was recrystallized from CH2Cl2 /hexane to yield 570 mg (90%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04892942 |
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| 출처 데이터셋 | uspto-grants-1990_01 |
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| ORD ID | ord-8c4ecdf71a2946e985d12e9cb2ad5e2c |
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| 출처 메모 | uspto-grants-1990_01 |
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