참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Methylcyclohexanone | HCID 11525 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ethyl 2-methoxyacetate | HCID 77544 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-(2-Methoxyacetyl)-4-methylcyclohexan-1-one | HCID 20034908 | 87.9% |
반응 단계
In 50 ml of benzene was suspended 2.5 g of 60% sodium hydride. While cooling the suspension, a mixture of 5.6 g of 4-methylcyclohexanone and 5.4 g of ethyl methoxyacetate was dropwise added thereto. After stirring at room temperature for 2 hours, 20 ml of water was added thereto and the pH was rendered 3 with concentrated hyrochloric acid. The benzene phase was separated and the aqueous phase was extracted with ether. The benzene solution and the ether solution were combined with each other followed by washing with a sodium chloride aqueous solution. After drying, the mixture was concentrated to give 7.4 g of crude 2-methoxyacetyl-4-methylcyclohexanone. The crude product was used at the following step. (2) 4-Cyano-2,3,5,6,7,8-hexahydro-1-methoxymethyl-7-methyl-3-oxoisoquinoline
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04845228 |
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| 출처 데이터셋 | uspto-grants-1989_07 |
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| ORD ID | ord-7d7e4b78548b4ce6aea6dafc1effcb5b |
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| 출처 메모 | uspto-grants-1989_07 |
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