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HCID 14497602, 화합물 → HCID 53740142, 화합물

HRID 373490
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HRID 373490 반응식
[CH3:1][Mg+].[Br-].[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[N:15]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=3)[N:14]=[C:13]([CH2:24][CH2:25][C:26](=[O:28])[CH3:27])[CH:12]=2)=[CH:7][CH:6]=1>C1COCC1>[Cl:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[N:15]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=3)[N:14]=[C:13]([CH2:24][CH2:25][C:26]([OH:28])([CH3:1])[CH3:27])[CH:12]=2)=[CH:9][CH:10]=1
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참가 물질

4

반응물 2

HCID 14497602HCID 14497602, 화합물HCID 178418689HCID 178418689, 화합물

생성물 1

HCID 53740142HCID 53740142, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of MeMgBr (1.32 ml of 3.2M, 4.23 mM) in THF (15 ml) at 0° C., was added a solution of the ketone 23, (1.00 g, 2.82 mM) in THF (25 ml) dropwise over a 20 minute period. After stirring for 1 hour, the reaction mixture was quenched with a saturated NH4Cl solution, diluted to a 100 ml volume with Et2O, washed with H2O, dried (Na2SO4), filtered, and concentrated in vacuo. Chromatography of the residue (Baker silica gel, 45 g) with Et2O as eluent, afforded 27, (0.68 g, 80% corrected for recovered starting material) as a colorless oil.

후처리

  1. customthe reaction mixture was quenched with a saturated NH4Cl solution
  2. additiondiluted to a 100 ml volume with Et2O
  3. washwashed with H2O
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customChromatography of the residue (Baker silica gel, 45 g) with Et2O as eluent, afforded
  8. custom27, (0.68 g, 80% corrected for recovered starting material) as a colorless oil

출처 및 근거

ORD 기록
ord-6f7a1f13af5b4f2483a7aca359ac6814
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05164381

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