1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 2-amino-2-methyl-N-(methylsulphonyl)benzamide

HRID 245340

반응식

HRID 245340 반응식
[NH2:1][C:2]1[C:10](C)=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH3:12][S:13]([NH2:16])(=[O:15])=[O:14].[CH2:17](N=C=NCCCN(C)C)C>ClCCl.CN(C)C1C=CN=CC=1>[NH2:1][C:2]1([CH3:17])[CH:10]=[CH:9][CH:8]=[CH:7][CH:3]1[C:4]([NH:16][S:13]([CH3:12])(=[O:15])=[O:14])=[O:6]

참가 물질

6

반응물 3

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 72879MethanesulfonamideHCID 781012-Amino-3-methylbenzoic acid

생성물 1

HCID 866602642-amino-2-methyl-N-(methylsulphonyl)benzamide

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

20 g (128 mmol) of 2-amino-3-methylbenzoic acid are dissolved in 600 ml of dichloromethane, and 10.98 g (115 mmol) of methanesulphonamide, 24.40 g (154 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 15.68 g (128 mmol) of 4-(dimethylamino)pyridine are then added under argon. The reaction is stirred at room temperature for 16 h, the solvent is distilled off and the residue is taken up in ethyl acetate and water. The ethyl acetate phase is washed four times with a 1N hydrochloric acid solution and then in each case once with water and a concentrated sodium chloride solution. After drying over sodium sulphate, the desired product is obtained by chromatographic purification.

후처리

  1. distillationthe solvent is distilled off
  2. washThe ethyl acetate phase is washed four times with a 1N hydrochloric acid solution
  3. dry with materialAfter drying over sodium sulphate

출처 및 근거

ORD 기록
ord-309219c488304383992fdc092b007281
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658800B2

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