참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 반응물 | 3-(4-Chlorophenoxy)-2-butanone | HCID 3722632 | — |
| 반응물 | Sodium cyanoborohydride | HCID 5003444 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2-(4-Chlorophenoxy)-1-methylpropylamine | HCID 18972724 | 86% |
반응 단계
82 g of ammonium acetate and 6.7 g of sodium cyanoborohydride were added to a solution containing 21 g of 3-(4-chlorophenoxy)-2-butanone dissolved in 500 mL of methanol, and the reaction mixture was stirred for 20 hours at room temperature. The reaction mixture was then concentrated under reduced pressure, and 180 mL of concentrated hydrochloric acid and 100 mL of water were added to the residue. The whole mixture was extracted with 300 mL of diethyl ether. The obtained water layer was alkalifled using a 5% aqueous solution of sodium hydroxide, and then extracted with 500 mL of ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. A fraction possessing a low boiling point was removed from the obtained oily products to afford 18 g (yield 86%) of the desired product. Refractive index: 1.5360.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05723469 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
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| ORD ID | ord-af2de60e1e754abb8358597255083dbf |
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| 출처 메모 | uspto-grants-1998_03 |
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