Ammonia → N-BENZYLIDENE-2-PROPYNYLAMINE

HRID 1292540노트

반응식

HRID 1292540 반응식
CS(O[CH2:6][C:7]#[CH:8])(=O)=O.[CH:9](=O)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[NH3:17]>C1(C)C=CC=CC=1>[CH:9](=[N:17][CH2:6][C:7]#[CH:8])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 240BenzaldehydeHCID 305925propargyl mesylate

생성물 1

HCID 4172560N-BENZYLIDENE-2-PROPYNYLAMINE수율 80%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Propargyl methanesulfonate (46.8 g, 0.35 mol) and benzaldehyde (47.0 g, 0.44 mol) were dissolved in 148 g of toluene and an aqueous 28% ammonia solution (180 g, 2.96 mol) was added dropwise at 24° C. over 7.5 hours to the solution, followed by stirring at the same temperature for 15 hours. After separating, the resultant organic phase was washed with water and concentrated to obtain 56.5 g of a crude product containing 40.0 g (yield: 80%) of N-benzylidene-2-propynylamine. The resulting crude product was distilled to obtain 34.9 g (purity: 97%, boiling point: 80°-83° C./2.5 mmHg) of N-benzylidene-2-propylamine.

후처리

  1. customAfter separating
  2. washthe resultant organic phase was washed with water
  3. concentrationconcentrated
  4. customto obtain 56.5 g of a crude product

출처 및 근거

ORD 기록
ord-a2f1271f7bb146ddb009283fd45d65be
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05756769

반응 노트

불러오는 중…