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Methanol → HCID 14722453, 화합물

HRID 1031667
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HRID 1031667 반응식
Br[CH:2]1[C:7](=[O:8])[C:6]2[CH:9]=[C:10]([O:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:11]([NH:13][S:14]([CH3:17])(=[O:16])=[O:15])=[CH:12][C:5]=2[O:4][CH2:3]1.[CH3:25][OH:26]>F[B-](F)(F)F.[Ag+]>[CH3:25][O:26][CH:2]1[C:7](=[O:8])[C:6]2[CH:9]=[C:10]([O:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:11]([NH:13][S:14]([CH3:17])(=[O:16])=[O:15])=[CH:12][C:5]=2[O:4][CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 887MethanolHCID 10621601HCID 10621601, 화합물

생성물 1

HCID 14722453HCID 14722453, 화합물수율 35%

시약·촉매·용매 1

HCID 159722Silver tetrafluoroborate촉매

실험 절차

There were mixed 4.12 g of 3-bromo-2,3-dihydro-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one, 9.37 g of silver tetrafluoroborate and 100 ml of methanol. The mixture was refluxed for 4 hours. The reaction mixture was cooled and filtered to remove the insolubles. The filtrate was subjected to distillation under reduced pressure to remove the solvent. The residue was purified by a column chromatography (eluant: a 5 : 1 mixture of toluene and ethyl acetate) to obtain 1.27 g (yield: 35%) of 2,3-dihydro-3-methoxy-7-methylsulfonylamino-6-phenoxy-4H-1-benzopyran-4-one.

후처리

  1. temperatureThe mixture was refluxed for 4 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. customto remove the insolubles
  5. distillationThe filtrate was subjected to distillation under reduced pressure
  6. customto remove the solvent
  7. customThe residue was purified by a column chromatography (eluant
  8. additiona 5 : 1 mixture of toluene and ethyl acetate)

출처 및 근거

ORD 기록
ord-3236888891234dd3bdc986e52efe8ff2
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04954518

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