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Cesium carbonate → HCID 86697127, 화합물

HRID 237555
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인쇄 미리보기

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HRID 237555 반응식
[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([OH:9])=[CH:4][C:3]=1[CH3:10].C([O-])([O-])=O.[Cs+].[Cs+].[CH3:17][C:18]1([CH3:25])[CH2:23]OS(=O)[O:20][CH2:19]1>CN(C)C=O>[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([O:9][CH2:17][C:18]([CH3:25])([CH3:23])[CH2:19][OH:20])=[CH:4][C:3]=1[CH3:10]
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참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 819704-Bromo-3,5-dimethylphenolHCID 108772945,6-Dihydro-5,5-dimethyl-4H-1,3,2-dioxathiin 2-oxide

생성물 1

HCID 86697127HCID 86697127, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

To a mixture of 4-bromo-3,5-dimethylphenol (625 mg) and Cs2CO3 (5 g) in N,N-dimethylformamide (10 mL) is added 5,5-dimethyl-[1,3,2]dioxathiane-2-oxide (467 mg). The mixture is stirred for 12 hours at 100° C. and then partitioned between water and ethyl acetate. The organic phase is washed with brine and dried (MgSO4). The solvent is evaporated and the residue is purified by HPLC on reversed phase to give the title compound. Yield: 251 mg; LC (method 7): tR=1.16 min; Mass spectrum (ESI+): m/z=287 [M+H]+.

후처리

  1. custompartitioned between water and ethyl acetate
  2. washThe organic phase is washed with brine
  3. dry with materialdried (MgSO4)
  4. customThe solvent is evaporated
  5. customthe residue is purified by HPLC on reversed phase

출처 및 근거

ORD 기록
ord-a84d3eee0aec43e6a0190e2bef892f7e
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08642585B2

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