참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Formaldehyde | HCID 712 | — |
| 반응물 | 5-Methyl-2-hexanone | HCID 8034 | — |
| 반응물 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-((Dimethylamino)methyl)-5-methyl-2-hexanone | HCID 53419039 | 16% |
반응 단계
Dimethylamine HCl (90 g, 1.1 mol), 5-methyl-2-hexanone (450 mL, 3.3 mol), and paraformaldehyde (50 g, 1.7 mol) were suspended in MeOH (80 mL) and concentrated HCl (200 μL) was added. The reaction mixture was heated to 80° C. for 12 hours. The mixture was allowed to cool to room temperature and 10% NaOH was added until basic. The entire mixture was extracted with Et2O (100 mL, 2×). The organic layer was dried over MgSO4 and concentrated. The crude reaction mixture was columned via flash column chromatography (0.5:9.5 MeOH:CH2Cl2) to give 30 g (175 mmol) of 3-dimethylaminomethyl-5-methyl-hexan-2-one 1a in a 16% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08039627B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_10 |
|---|
| ORD ID | ord-86428a6221074dd6b4cd608150d4bbf0 |
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| 출처 메모 | uspto-grants-2011_10 |
|---|
