참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Benzyl chloroformate | HCID 10387 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 4-Piperidinecarboxylic acid, 4-phenyl-, 4-methylbenzenesulfonate (1:1) | HCID 2723657 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | 1-(Benzyloxycarbonyl)-4-phenylpiperidine-4-carboxylic acid | HCID 22741798 | 90.3% |
반응 단계
A mixture of 37.7 g of 4-carboxy-4-phenylpiperidine p-toluenesulfonate, 53.3 g of 30% aqueous NaOH solution and 250 ml of water is cooled to 5° C. A solution of 18 g of benzyl chloroformate in 60 ml of acetone is added rapidly at 5° C. and the reaction mixture is stirred overnight, the temperature being allowed to rise to RT. It is washed twice with ether and, after decantation, the aqueous phase is acidified to pH 1 by the addition of concentrated HCl and then 2 N HCl. The precipitate formed is filtered off, dried, taken up with ether and filtered off again to give 30.6 g of the expected product, m.p.=142-144° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06710042B2 |
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| 출처 데이터셋 | uspto-grants-2004_03 |
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| ORD ID | ord-bc0f94f9e9c1453c86a8f5411fc78675 |
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| 출처 메모 | uspto-grants-2004_03 |
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