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Dichloromethane → HCID 66834653, 화합물

HRID 2275288
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HRID 2275288 반응식
C(Cl)Cl.C[O:5][C:6]1[CH:7]=[CH:8][C:9]2[C:21](=[O:22])[C:20]3[C:19]4[CH:18]=[CH:17][N:16]=[CH:15][C:14]=4[O:13][C:12]=3[C:11]([CH3:24])([CH3:23])[C:10]=2[CH:25]=1.B(Br)(Br)Br.C(=O)(O)[O-].[Na+]>O>[OH:5][C:6]1[CH:7]=[CH:8][C:9]2[C:21](=[O:22])[C:20]3[C:19]4[CH:18]=[CH:17][N:16]=[CH:15][C:14]=4[O:13][C:12]=3[C:11]([CH3:23])([CH3:24])[C:10]=2[CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

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6

반응물 4

HCID 6344Dichloromethane2회HCID 25134Boron tribromideHCID 516892Sodium BicarbonateHCID 668347578-Methoxy-10,10-dimethyl-10H-11-oxa-2-aza-benzo[b]fluoren-5-one

생성물 1

HCID 66834653HCID 66834653, 화합물수율 99.8%

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

DCM (0.34 ml) solution of 8-methoxy-10,10-dimethyl-10H-11-oxa-2-aza-benzo[b]fluoren-5-one (Compound GT15-11, 10 mg) was cooled to −78° C., added with the DCM solution (0.17 ml) of 1.0 M BBr3, and the mixture was stirred at room temperature overnight. To the reaction mixture, water and saturated aqueous solution of sodium bicarbonate were added, and the solid produced therefrom was filtered off. The filtrate was extracted with the mixture solution of DCM and MeOH (DCM:MeOH=9:1). The organic layer was washed with saturated brine. The filtered solid and the residues obtained after concentration under reduced pressure were combined to obtain the title compound (9.5 mg, 99%).

후처리

  1. customthe solid produced
  2. filtrationtherefrom was filtered off
  3. extractionThe filtrate was extracted with the mixture solution of DCM and MeOH (DCM:MeOH=9:1)
  4. washThe organic layer was washed with saturated brine
  5. customThe filtered solid and the residues obtained
  6. concentrationafter concentration under reduced pressure

출처 및 근거

ORD 기록
ord-3ff5a52da46d4e5ca23e95befafb383d
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09126931B2

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