Cesium carbonate → HCID 67316436, 화합물

HRID 1013299노트

반응식

HRID 1013299 반응식
[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[NH:6]2.Br[CH2:17][CH2:18][CH2:19][O:20][C:21]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:24]=[CH:23][CH:22]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C)C=O.CCOCC.O>[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:6]2[CH2:17][CH2:18][CH2:19][O:20][C:21]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:24]=[CH:23][CH:22]=1

참가 물질

7

반응물 3

HCID 10796Cesium carbonateHCID 10989255Ethyl 4-bromo-1H-indole-2-carboxylateHCID 129593811-(3-Bromopropoxy)naphthalene

생성물 1

HCID 67316436HCID 67316436, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of EXAMPLE 106A (5.5 g) in N,N-dimethylformamide (60 mL) was added 1-(3-bromopropoxy)naphthalene (5.4 g) and Cs2CO3 (22 g). The mixture was stirred overnight at room temperature. The mixture was diluted with ether (300 mL) and water (200 mL). The aqueous layer was extracted with ether twice. The combined extracts were washed with water (×3), brine and dried over Na2SO4. Concentration of the mixture gave crude product, which was purified by flash chromatography (2% ethyl acetate in hexane).

후처리

  1. extractionThe aqueous layer was extracted with ether twice
  2. washThe combined extracts were washed with water (×3), brine
  3. dry with materialdried over Na2SO4
  4. customConcentration of the mixture gave crude product, which
  5. customwas purified by flash chromatography (2% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-359af53542db48a599fdc39dd39560bc
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981888B2

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