참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Formaldehyde | HCID 712 | — |
| 반응물 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 반응물 | 3',4',5'-Trimethoxyacetophenone | HCID 14345 | — |
| 용매 | Acetone | HCID 180 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 3-(Dimethylamino)-1-(3,4,5-trimethoxyphenyl)propan-1-one | HCID 412306 | — |
반응 단계
Concentrated hydrochloric acid (1 mL) was added to a stirred mixture of 3,4,5-trimethoxyacetophenone (210 g, 1 mole), dimethylamine hydrochloride (81 g, 1 mole) and paraformaldehyde (45 g, 1.5 mole) in ethanol (300 mL). The reaction mixture was heated under reflux for 1 hour. Another portion of paraformaldehyde (30 g, 1 mole) was added, and the heating was continued for another 2 hours. The warm reaction mixture was poured with vigorous stirring into acetone (2.4 L). The slurry was heated at 60° C. for 15 minutes, cooled, and filtered. The solid was washed with acetone and dried to provide the hydrochloride salt of 3-(N,N-dimethylamino)-1-(3,4,5-trimethoxyphenyl)propan-1-one, R, 0.05 (SiO2, 2:1 [v/v] hexane-ethyl acetate); m.p. 175° C. A mixture of the above hydrochloride (147.5 g, 0.48 mole) in 1 N NaOH (750 mL) was shaken with ethyl acetate (4×100 mL). The combined organic extracts were washed with brine, dried, and evaporated in vacuo to provide 3-(N,N-dimethylamino)-1-(3,4,5-trimethoxyphenyl)propan-1-one.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05010100 |
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| 출처 데이터셋 | uspto-grants-1991_04 |
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| ORD ID | ord-e1b069017dad44c49678d1695b56f89a |
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| 출처 메모 | uspto-grants-1991_04 |
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