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Potassium Carbonate → HCID 68523343, 화합물

HRID 1992351
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인쇄 미리보기

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HRID 1992351 반응식
Br[CH2:2][CH2:3][NH:4][S:5]([C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=1)(=[O:7])=[O:6].[C:15]([O:19][C:20]([N:22]1[CH2:29][CH:28]2[O:30][CH:24]([CH2:25][NH:26][CH2:27]2)[CH2:23]1)=[O:21])([CH3:18])([CH3:17])[CH3:16].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[C:15]([O:19][C:20]([N:22]1[CH2:23][CH:24]2[O:30][CH:28]([CH2:27][N:26]([CH2:2][CH2:3][NH:4][S:5]([C:8]3[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=3)(=[O:7])=[O:6])[CH2:25]2)[CH2:29]1)=[O:21])([CH3:18])([CH3:16])[CH3:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

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HCID 11430Potassium CarbonateHCID 2779738N-(2-bromoethyl)-4-fluorobenzenesulfonamideHCID 185404123-Boc-9-oxa-3,7-diazabicyclo[3.3.1]nonane

생성물 1

HCID 68523343HCID 68523343, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
60 °C

실험 절차

A suspension of N-(2-Bromo-ethyl)-4-fluoro-benzenesulfonamide (7 g, 0.0179 mol; see step (i) above) and 9-oxa-3,7-diaza-bicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester (11.2 g, 0.159 mol; see WO 01/28992) and K2CO3 (9.7 g, 0.0798 mol) in dry acetonitrile (70 ml) was stirred at 60° C. overnight under nitrogen atmosphere. The reaction mixture was partitioned between brine and ethyl acetate. Organic layer was washed with brine and dried over sodium sulfate. Solvent evaporation under reduced pressure followed by column chromatography over silica gel using 7% ethyl acetate in petroleum ether as eluent afforded the sub-title compound as a solid. Yield: 4 g

후처리

  1. customThe reaction mixture was partitioned between brine and ethyl acetate
  2. washOrganic layer was washed with brine
  3. dry with materialdried over sodium sulfate
  4. customSolvent evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-0dd497de678b4d41a180dc8c20451ba6
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07648985B2

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