N,N-dimethyl-2-Furanmethanamine → HCID 20199141、化合物

HRID 652109

反応式

HRID 652109 の反応式
[CH3:1][N:2]([C:11](SC)=[N:12][C:13](=O)[CH2:14][S:15]([CH3:18])(=[O:17])=[O:16])[N:3]=CC1C=CC=CC=1.[CH3:22][N:23]([CH3:30])[CH2:24][C:25]1[O:26][CH:27]=[CH:28][CH:29]=1>C(#N)C>[CH3:22][N:23]([CH2:24][C:25]1[O:26][C:27]([CH2:18][S:15][CH2:14][CH2:13][NH:12][C:11]2[N:2]([CH3:1])[N:3]=[C:13]([CH2:14][S:15]([CH3:18])(=[O:16])=[O:17])[N:12]=2)=[CH:28][CH:29]=1)[CH3:30]

参加物

4

反応物 2

HCID 84478N,N-dimethyl-2-FuranmethanamineHCID 70434558HCID 70434558、化合物

生成物 1

HCID 20199141HCID 20199141、化合物収率 135.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

Methyl 1-methyl-N-[(methylsulphonyl)acetyl]-2-(phenylmethylene)hydrazinecarboximidothioate (1.05 g) and 5-[[2-aminoethyl)thio]methyl]-N,N-dimethylfuranmethanamine (0.85 g)in acetonitrile (3 ml) were heated on a steam bath at atmospheric pressure for 5 minutes then under water vacuum for 10 minutes. The oily residue was dissolved in acetonitrile (3 ml) and the solution re-evaporated under water vacuum. The oily residue was dissolved in 2N hydrochloric acid (3 ml) and 5N hydrochloric acid (4 ml) added to the solution. The solution was heated on a steam bath for 15 minutes and after cooling to room temperature, water (10 ml) was added and the oily suspension extracted with ethyl acetate. The aqueous phase was basified with sodium carbonate and the oily suspension extracted with ethyl acetate to yield an oil (0.84 g). This was chromatographed (using solvent system D) to give the title compound (0.78 g) as an oil. T.l.c. System D, Rf 0.5.

後処理

  1. customthe solution re-evaporated under water vacuum
  2. dissolutionThe oily residue was dissolved in 2N hydrochloric acid (3 ml)
  3. addition5N hydrochloric acid (4 ml) added to the solution
  4. temperatureThe solution was heated on a steam bath for 15 minutes
  5. additionwater (10 ml) was added
  6. extractionthe oily suspension extracted with ethyl acetate
  7. extractionthe oily suspension extracted with ethyl acetate

出典と根拠

ORDレコード
ord-5aa710dd1dd7493a801e0d6426adbcce
出典データセット
uspto-grants-1987_06
特許番号
US04670448

関連ノート

読み込み中…