N-Ethylethylenediamine → HCID 20225356、化合物

HRID 463683

反応式

HRID 463683 の反応式
[CH2:1]([NH:3][CH2:4][CH2:5][NH2:6])[CH3:2].[CH3:7][S:8]([NH:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([Cl:18])=[O:17])=[CH:14][CH:13]=1)(=[O:10])=[O:9]>O1CCCC1>[ClH:18].[CH2:1]([NH:3][CH2:4][CH2:5][NH:6][C:16](=[O:17])[C:15]1[CH:19]=[CH:20][C:12]([NH:11][S:8]([CH3:7])(=[O:10])=[O:9])=[CH:13][CH:14]=1)[CH3:2]

参加物

4

実験手順

To a solution of 4.45 g (50.5 mmoles) of N-ethylethylenediamine in 50 ml of tetrahydrofuran cooled in an ice/ethanol bath under a nitrogen atmosphere add dropwise a solution of 11.8 g (50.5 mmoles) of 4-[(methylsulfonyl)amino]benzoyl chloride in 100 ml of tetrahydrofuran. When the addition is complete, allow the mixture to warm to room temperature and stir overnight. Filter the resulting solid and wash the solid with tetrahydrofuran then with diethyl ether. Triturate the solid in acetone, then recrystallize from 90% aqueous methanol to obtain the title compound.

後処理

  1. additionWhen the addition
  2. filtrationFilter the resulting solid
  3. washwash the solid with tetrahydrofuran
  4. customTriturate the solid in acetone
  5. customrecrystallize from 90% aqueous methanol

出典と根拠

ORDレコード
ord-48aa1403aa7244b387efc142af8ece4f
出典データセット
uspto-grants-1985_10
特許番号
US04544654

関連ノート

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