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Pyridine → HCID 56966058, 화합물

HRID 1036934
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HRID 1036934 반응식
[CH3:1][C:2]1([CH3:20])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH3:12])[CH:10]=2)[NH:5][CH:4]([C:13]2[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=2[NH2:15])[CH2:3]1.N1C=CC=CC=1.[CH3:27][S:28](Cl)(=[O:30])=[O:29]>ClCCl.O>[CH3:1][C:2]1([CH3:20])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH3:12])[CH:10]=2)[NH:5][CH:4]([C:13]2[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=2[NH:15][S:28]([CH3:27])(=[O:30])=[O:29])[CH2:3]1
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참가 물질

6

반응물 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 67291611HCID 67291611, 화합물

생성물 1

HCID 56966058HCID 56966058, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-(4,4,6-trimethyl-1,2,3,4-tetrahydroquinolin-2-yl)aniline (150 mg, 0.56 mmol) and pyridine (0.5 mL) in anhydrous dichloromethane (2 mL) was added methanesulfonyl chloride (44 μL) at ice-bath under nitrogen. After addition, the resulting mixture was stirred at room temperature for 3 h. The reaction mixture was diluted with water, and extracted with ethyl acetate. The combined organic layer was dried over anhydrous Sodium sulfate, and then concentrated. The residue was purified by HPLC to give N-[2-(4,4,6-trimethyl-1,2,3,4-tetrahydro-quinolin-2-yl)-phenyl]methanesulfonamide LC/MS m/e obsd. (ESI+) [(M+H)+] 345.2.

후처리

  1. additionAfter addition
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organic layer was dried over anhydrous Sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by HPLC

출처 및 근거

ORD 기록
ord-1179e13da73e4f3aa5303a92cb91a327
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08546427B2

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