関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Tributylstannane | HCID 5948 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 4-t-Butyl 7beta-t-butyloxycarbonylamino-3-allyloxycarbonyl-1-carba-3-cephem-4-carboxylate | HCID 14281586 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Acetonitrile ether | HCID 21885917 | — |
| 生成物 | HCID 14854210 | HCID 14854210 | 90% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04892942 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-8c4ecdf71a2946e985d12e9cb2ad5e2c |
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| 出典メモ | uspto-grants-1990_01 |
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