Ammonia → N-BENZYLIDENE-2-PROPYNYLAMINE

HRID 1292540ノート

反応式

HRID 1292540 の反応式
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

参加物

5

反応物 3

HCID 222AmmoniaHCID 240BenzaldehydeHCID 305925propargyl mesylate

生成物 1

HCID 4172560N-BENZYLIDENE-2-PROPYNYLAMINE収率 80%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-a2f1271f7bb146ddb009283fd45d65be
出典データセット
uspto-grants-1998_05
特許番号
US05756769

反応ノート

読み込み中…