Benzaldehyde → HCID 14010268、化合物

HRID 1731772ノート

反応式

HRID 1731772 の反応式
[ClH:1].[CH3:2][N:3]([CH3:11])[S:4]([NH:7][CH2:8][CH2:9][NH2:10])(=[O:6])=[O:5].[CH:12](=O)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(N(CC)CC)C>C1C=CC=CC=1>[ClH:1].[CH:12](=[N:10][CH2:9][CH2:8][NH:7][S:4]([N:3]([CH3:11])[CH3:2])(=[O:6])=[O:5])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 240BenzaldehydeHCID 8471TriethylamineHCID 14010266[(2-Aminoethyl)sulfamoyl]dimethylamine hydrochloride

生成物 1

HCID 14010268HCID 14010268、化合物収率 50%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

A mixture of 4.0 g (0.02 mole) of 2-[N-[(dimethylamino)sulfonyl]amino]ethylamine hydrochloride and 2.0 g (0.02 mole) of benzaldehyde was stirred and treated immediately with 2.0 g (0.02 mole) of triethylamine, followed by the addition of 200 ml of dry benzene. The solution was heated to reflux employing a Dean-Stark apparatus. After 2 hr at reflux, the benzene solution was cooled and washed twice with 100 ml portions of water. The organic phase was separated, dried over magnesium sulfate, and concentrated under reduced pressure to an oil, which was dissolved in ether and treated with HCl gas to precipitate a yellowish solid. The product was collected by filtration, washed with ether and air dried to provide 2.4 g (50%) of product. The NMR spectrum was consistent with the assigned structure and the solid was used without additional purification.

後処理

  1. temperatureThe solution was heated
  2. temperatureto reflux
  3. temperatureAfter 2 hr at reflux
  4. washwashed twice with 100 ml portions of water
  5. customThe organic phase was separated
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure to an oil, which
  8. dissolutionwas dissolved in ether
  9. additiontreated with HCl gas
  10. customto precipitate a yellowish solid
  11. filtrationThe product was collected by filtration
  12. washwashed with ether and air
  13. customdried

出典と根拠

ORDレコード
ord-5d7a066656ad4148b5dcf1a013b76652
出典データセット
uspto-grants-1986_11
特許番号
US04623652

反応ノート

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