Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethanolamine → 2,2-Dichloro-1-(8-methyl-1-oxa-4-azaspiro[4.5]decan-4-yl)ethan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethanolamine | HCID 700 | — |
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Dichloroacetyl chloride | HCID 6593 | — |
| 반응물 | 4-Methylcyclohexanone | HCID 11525 | — |
| 생성물 | 2,2-Dichloro-1-(8-methyl-1-oxa-4-azaspiro[4.5]decan-4-yl)ethan-1-one | HCID 13277204 | — |
반응 단계
From a boiling mixture of 11.2 g. (0.1 moles) of 4-methyl-cyclohexanone and 6.1 g. (0.1 moles) of ethanolamine in 100 ml. of benzene the formed water is continuously distilled off. Boiling is continued until 1.8 ml. of water are separated. The reaction mixture is then cooled and 8 g. (0.1 moles) of pyridine are added followed by dropwise addition of 14.7 g. (0.1 moles) of dichloroacetyl chloride with external salt/ice cooling. Further following the procedure described in Example 2, 20.7 g. (0.078 moles) of a rose, oily product are obtained. Recrystallization from absolute ethanol affords a white, crystalline product melting at 119° to 120° C. The structure of the compound obtained can be verified by IR spectrum analysis.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04256481 |
| 출처 데이터셋 | uspto-grants-1981_03 |
| ORD ID | ord-7e8eee49de1241f0a4981066e19cc3e7 |
| 출처 메모 | uspto-grants-1981_03 |