Formaldehyde → 5-{[N-methyl-N-(2-propynyl)amino]methyl}-2-furanmethanol
반응식
[CH2:1]([OH:7])[C:2]1[O:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH3:9][NH:10][CH2:11][C:12]#[CH:13].[CH2:14]=O.[OH-].[Na+]>>[CH3:9][N:10]([CH2:14][C:5]1[O:6][C:2]([CH2:1][OH:7])=[CH:3][CH:4]=1)[CH2:11][C:12]#[CH:13]참가 물질
5
실험 절차
To furfuryl alcohol (2.49 g; 25.4 mmoles) which was cooled in an ice-water bath to 5° was added N-methylpropargylamine hydrochloride (4.0 g; 37.9 mmoles) and 40% formalin (3.13 ml; 41.7 mmoles), and the mixture stirred while allowed to reach ambient temperature. After 1 hour of stirring the solution was allowed to stand at ambient temperature for 41/2 days. The reaction mixture was poured into ice water, made strongly basic with 40% aqueous NaOH and extracted with five portions of methylene chloride. The combined organic phase was dried, filtered and evaporated under reduced pressure to give the product as an oil (quantitative yield). Vacuum distillation yielded the title compound, bp 102°-106°/0.3 mm Hg.
후처리
- customto reach ambient temperature
- stirringAfter 1 hour of stirring the solution
- customto stand at ambient temperature for 41
- custom2 days
- extractionextracted with five portions of methylene chloride
- customThe combined organic phase was dried
- filtrationfiltered
- customevaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-72453b8651fe4d4fa2c0d0ea5a3c17d4
- 출처 데이터셋
- uspto-grants-1983_07
- 특허 번호
- US04394508
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