Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylamine → 4-Dimethylaminomethyl-5-(3-methoxyphenyl)-1-phenylpyrrolidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylamine | HCID 674 | — |
| 반응물 | 5-(3-Methoxyphenyl)-1-phenyl-4-(p-toluenesulfonyloxymethyl)pyrrolidin-2-one | HCID 13362004 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-Dimethylaminomethyl-5-(3-methoxyphenyl)-1-phenylpyrrolidin-2-one | HCID 13362005 | — |
반응 단계
To 22.0 gm. of 5-(3-methoxyphenyl)-1-phenyl-4-(p-toluenesulfonyloxymethyl)pyrrolidin-2-one in 150 ml. of dimethylformamide was added 21 ml. of 40% aqueous dimethylamine, the solution refluxed for 3 hours and then 21 ml. more of 40% aqueous dimethylamine added and reflux continued for an additional 3 hours. After cooling the reaction was decanted into ice water and acidified. Extraction with ether followed by basification of the aqueous phase with potassium carbonate yielded a semi-solid which was extracted with chloroform, dried (Na2SO4), filtered and concentrated in vacuo to a solid. Recrystallization from acetonitrile provided 7.0 gm. of beige crystals, m.p. 88°-92°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04639529 |
| 출처 데이터셋 | uspto-grants-1987_01 |
| ORD ID | ord-d565591e3d194d16aa95970b043eccb3 |
| 출처 메모 | uspto-grants-1987_01 |