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2-Dimethylaminopyridine → HCID 135544176, 화합물

HRID 496009
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HRID 496009 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([S:10](Cl)(=[O:12])=[O:11])=[CH:6][C:5]=1[C:14]1[NH:19][C:18](=[O:20])[C:17]2=[C:21]([CH3:29])[N:22]=[C:23]([CH:24]([CH2:27][CH3:28])[CH2:25][CH3:26])[N:16]2[N:15]=1)[CH3:2].CN(C1C=CC=CN=1)C.[CH3:39][N:40]1[CH2:45][CH2:44][NH:43][CH2:42][CH2:41]1>ClCCl>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([S:10]([N:43]2[CH2:44][CH2:45][N:40]([CH3:39])[CH2:41][CH2:42]2)(=[O:12])=[O:11])=[CH:6][C:5]=1[C:14]1[NH:19][C:18](=[O:20])[C:17]2=[C:21]([CH3:29])[N:22]=[C:23]([CH:24]([CH2:27][CH3:28])[CH2:25][CH3:26])[N:16]2[N:15]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 218852-DimethylaminopyridineHCID 531671-MethylpiperazineHCID 135552977HCID 135552977, 화합물

생성물 1

HCID 135544176HCID 135544176, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

50 mg (0.114 mmol) of 4-ethoxy-3-(5-methyl-4-oxo-7-(1-ethylpropyl)-3,4-dihydro-imidazo[5,1-f][1,2,4]triazin-2-yl)-benzenesulphonyl chloride are initially charged in 5 ml of dichloromethane and a spatula tip of 4 dimethylaminopyridine is added, followed by 30 mg (0.342 mmol) of N-methylpiperazine. The mixture is stirred at room temperature overnight, diluted with dichloromethane, washed twice with saturated ammonium chloride solution, dried over sodium sulphate, concentrated and filtered through silica gel (methanol).

후처리

  1. washwashed twice with saturated ammonium chloride solution
  2. dry with materialdried over sodium sulphate
  3. concentrationconcentrated
  4. filtrationfiltered through silica gel (methanol)

출처 및 근거

ORD 기록
ord-bb118e038fac4cafa93e964d39290571
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06943163B2

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