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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Pyridine → N-[3-(4-butyl-1-hydroxy-4-methyl-3-oxo-2-naphthyl)-1,1-dioxo-4H-1$l^{6},2,4-benzothiadiazin-7-yl]methanesulfonamide

HRID 494529
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인쇄 미리보기

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HRID 494529 반응식
Cl.[NH2:2][C:3]1[CH:31]=[CH:30][C:6]2[NH:7][C:8]([C:13]3[C:14](=[O:29])[C:15]([CH2:25][CH2:26][CH2:27][CH3:28])([CH3:24])[C:16]4[C:21]([C:22]=3[OH:23])=[CH:20][CH:19]=[CH:18][CH:17]=4)=[N:9][S:10](=[O:12])(=[O:11])[C:5]=2[CH:4]=1.[S:32](Cl)([CH3:35])(=[O:34])=[O:33].N1C=CC=CC=1>CC(C)=O>[CH2:25]([C:15]1([CH3:24])[C:16]2[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:22]([OH:23])=[C:13]([C:8]2[NH:7][C:6]3[CH:30]=[CH:31][C:3]([NH:2][S:32]([CH3:35])(=[O:34])=[O:33])=[CH:4][C:5]=3[S:10](=[O:12])(=[O:11])[N:9]=2)[C:14]1=[O:29])[CH2:26][CH2:27][CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 1364037393-(7-Amino-1,1-dioxido-4h-1,2,4-benzothiadiazin-3-yl)-1-butyl-4-hydroxy-1-methylnaphthalen-2(1h)-one hydrochloride

생성물 1

HCID 135440188N-[3-(4-butyl-1-hydroxy-4-methyl-3-oxo-2-naphthyl)-1,1-dioxo-4H-1$l^{6},2,4-benzothiadiazin-7-yl]methanesulfonamide수율 96%

시약·촉매·용매 1

HCID 180
Acetone
용매

실험 절차

A solution of Example 33B (0.052 g, 0.112 mmol), mesyl chloride (0.035 mL, 0.447 mmol), and pyridine (0.073 mL, 0.893 mmol) in acetone (1.5 mL) was stirred at 25° C. for 18 hours. The solution was partitioned between ethyl acetate and dilute citric acid and the layers were separated. The ethyl acetate layer was dried with sodium sulfate, filtered, and concentrated in vacuo. The residue was chromatographed on silica gel eluting with methylene chloride and 2.5% methanol in methylene chloride to give the desired product (0.054 g, 96%).

후처리

  1. customThe solution was partitioned between ethyl acetate and dilute citric acid
  2. customthe layers were separated
  3. dry with materialThe ethyl acetate layer was dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was chromatographed on silica gel eluting with methylene chloride and 2.5% methanol in methylene chloride

출처 및 근거

ORD 기록
ord-98eb17253bb7421f96b5620482a61fe8
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07538105B2

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