N-Ethylethylenediamine → HCID 20225356, 화합물

HRID 463683

반응식

HRID 463683 반응식
[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]

참가 물질

4

반응물 2

HCID 66071N-EthylethylenediamineHCID 117911194-[(Methylsulfonyl)amino]benzoyl chloride

생성물 1

HCID 20225356HCID 20225356, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-48aa1403aa7244b387efc142af8ece4f
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04544654

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