참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | 4-(2,6,6-Trimethylcyclohex-2-en-1-ylidene)but-2-en-2-yl acetate | HCID 53406773 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 4-(2,6,6-Trimethyl-2-cyclohexen-1-ylidene)-butan-2-ol | HCID 53692157 | 107.2% |
반응 단계
The resulting crude acetoxy compound of formula II (108 g) is dissolved in 400 ml of ethanol (96%) and added dropwise within 10 minutes at 20°-30° C with slight cooling to a suspension of 20 g of sodium borohydride in 600 ml of 96% ethanol. The mixture is then heated until a slight reflux occurs and stirred at this temperature for 15 minutes. The end of the reaction can be detected by a spontaneous colour change from dark-yellow to lemon-yellow. After cooling to room temperature, the cloudy mixture is poured on to saturated ammonium chloride solution/ice and the mixture is extracted with hexane. After the usual washing to neutrality with water and drying over anhydrous sodium sulphate, the solvent is evaporated under a vacuum. There are obtained 96 g of crude 4-(2,6,6-trimethyl-2-cyclohexen-1-ylidene)-butan-2-ol (formula III).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04072719 |
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| 출처 데이터셋 | uspto-grants-1978_02 |
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| ORD ID | ord-14aeedd14fd4480ea6b33e5898f7eea6 |
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| 출처 메모 | uspto-grants-1978_02 |
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