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Triethylamine → HCID 44382365, 화합물

HRID 583933
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HRID 583933 반응식
[OH:1][C:2]1[CH:7]=[CH:6][N:5]([CH3:8])[C:4](=[O:9])[CH:3]=1.C(N(CC)CC)C.[CH3:17][O:18][C:19]1[CH:20]=[C:21]([S:29](Cl)(=[O:31])=[O:30])[CH:22]=[C:23]([O:27][CH3:28])[C:24]=1[O:25][CH3:26]>O1CCOCC1.CN(C=O)C.C(OCC)(=O)C>[CH3:28][O:27][C:23]1[CH:22]=[C:21]([S:29]([O:1][C:2]2[CH:7]=[CH:6][N:5]([CH3:8])[C:4](=[O:9])[CH:3]=2)(=[O:30])=[O:31])[CH:20]=[C:19]([O:18][CH3:17])[C:24]=1[O:25][CH3:26]
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참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 151961583,4,5-Trimethoxybenzene-1-sulfonyl chlorideHCID 546845234-Hydroxy-1-Methyl-1h-pyridin-2-one

생성물 1

HCID 44382365HCID 44382365, 화합물수율 36.9%

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate
용매
HCID 312751,4-Dioxane용매

실험 절차

A solution of 4-hydroxy-1-methyl-1H-pyridin-2-one ([40357-87-7], 44.9 mg, 0.358 mmol) in dioxane (2 mL) and DMF (1 mL) was treated with triethylamine (0.15 mL) and 3,4,5-trimethoxybenzenesulfonylchloride (97.1 mg, 0.358 mmol), stirred for 48 hours at room temperature, diluted with ethyl acetate, washed with 1.1M NaHSO4, dried (MgSO4), filtered and concentrated. Chromatography of the concentrate on silica gel with 40% ethyl acetate/hexane provided 47 mg of the desired compound.

후처리

  1. washwashed with 1.1M NaHSO4
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. concentrationChromatography of the concentrate on silica gel with 40% ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-bcb6abcd71154dd6bcba2e9f5c544371
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06924304B2

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