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Acetic Acid → HCID 19858061, 화합물

HRID 2073398
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HRID 2073398 반응식
Br[CH2:2][C:3]1[CH:15]=[C:14]2[C:6]([CH:7]=[C:8]([S:19]([CH3:22])(=[O:21])=[O:20])[C:9]3[O:10][C:11](=[O:18])[C:12]([CH3:17])([CH3:16])[C:13]=32)=[CH:5][C:4]=1[S:23]([CH3:26])(=[O:25])=[O:24].[NH:27]1[CH:31]=[N:30][CH:29]=[N:28]1.C(=O)([O-])[O-].[K+].[K+].C(O)(=O)C>C(#N)C.O>[S:19]([C:8]1[C:9]2[O:10][C:11](=[O:18])[C:12]([CH3:16])([CH3:17])[C:13]=2[C:14]2[C:6](=[CH:5][C:4]([S:23]([CH3:26])(=[O:24])=[O:25])=[C:3]([CH2:2][N:27]3[CH:31]=[N:30][CH:29]=[N:28]3)[CH:15]=2)[CH:7]=1)([CH3:22])(=[O:20])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 19858047HCID 19858047, 화합물

생성물 1

HCID 19858061HCID 19858061, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 6342
Acetonitrile
용매

실험 절차

A solution of 8-bromomethyl-4,7-dimesyl-1,1-dimethyl-2(1H)-naphtho[2,1-b]furanone in acetonitrile (5 ml) was treated with 1,2,4-triazole (0.2 g) and potassium carbonate (0.14 g), and the mixture was stirred under reflux for 18 h. The mixture was diluted with water, neutralised with glacial acetic acid and extracted with ethyl acetate, and the ethyl acetate extract was dried and evaporated to dryness under reduced pressure. The residue was purified by flash chromatography, using methanol:ethyl acetate, 1:99 v/v as eluant, to give 4,7-dimesyl-1,1-dimethyl-8-(1H-1,2,4-triazol-1-ylmethyl)-2(1H)-naphtho[2,1-b]furanone, m.p. 263°-264° after recrystallisation from ethyl acetate.

후처리

  1. temperatureunder reflux for 18 h
  2. extractionextracted with ethyl acetate
  3. extractionthe ethyl acetate extract
  4. customwas dried
  5. customevaporated to dryness under reduced pressure
  6. customThe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-4a01eabf4c114e979cc4eadd2e3674f0
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04916148

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