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Sodium hydride → 8-Methoxy-3,4-dihydro-2H-pyrido[2',3':4,5]pyrrolo[2,1-b][1,3]oxazine

HRID 1767565
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인쇄 미리보기

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HRID 1767565 반응식
[H-].[Na+].Br[CH2:4][CH2:5][CH2:6][N:7]1[C:15]2[C:10](=[N:11][C:12]([O:16][CH3:17])=[CH:13][CH:14]=2)[CH2:9][C:8]1=[O:18]>CN(C)C=O>[CH3:17][O:16][C:12]1[CH:13]=[CH:14][C:15]2[N:7]3[C:8]([O:18][CH2:4][CH2:5][CH2:6]3)=[CH:9][C:10]=2[N:11]=1
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참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 112661091-(3-Bromopropyl)-5-methoxy-1,3-dihydro-2H-pyrrolo[3,2-b]pyridin-2-one

생성물 1

HCID 114014538-Methoxy-3,4-dihydro-2H-pyrido[2',3':4,5]pyrrolo[2,1-b][1,3]oxazine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

Under an inert atmosphere, 160 mg (4 mmol) of sodium hydride (60% in oil) are added slowly at 0° C. to a solution of 380 mg (1.34 mmol) of the compound obtained in Step E in 10 ml of N,N-dimethylformamide. The reaction mixture is stirred at 0° C. for 30 minutes before being hydrolysed with ice and then extracted with ethyl acetate. The organic phase is washed several times with water, dried over magnesium sulphate, concentrated and purified by flash chromatography over silica gel (eluant:ethyl acetate/petroleum ether, 95:5) to yield the title compound in the form of a brown solid.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic phase is washed several times with water
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated
  5. custompurified by flash chromatography over silica gel (eluant:ethyl acetate/petroleum ether, 95:5)

출처 및 근거

ORD 기록
ord-051cca268af249c0b50816ac240b55d1
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07235550B2

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