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Diisopropylethylamine → HCID 118059329, 화합물

HRID 2279096
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HRID 2279096 반응식
[Na+].[CH3:2][C:3]1[C:11]2[C:10]([C:12]([O-:14])=O)=[CH:9][C:8]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH:22]4[CH2:27][CH2:26][CH2:25][CH2:24][O:23]4)=[CH:17][CH:16]=3)=[N:7][C:6]=2[N:5]([CH:28]2[CH2:33][CH2:32][CH2:31][CH2:30][O:29]2)[N:4]=1.CCN(C(C)C)C(C)C.[C:43]([O:47][C:48]([N:50]1[CH2:57][C:54]2([CH2:56][CH2:55]2)[NH:53][CH2:52][CH2:51]1)=[O:49])([CH3:46])([CH3:45])[CH3:44]>C(Cl)Cl.O>[C:43]([O:47][C:48]([N:50]1[CH2:57][C:54]2([CH2:55][CH2:56]2)[N:53]([C:12]([C:10]2[C:11]3[C:3]([CH3:2])=[N:4][N:5]([CH:28]4[CH2:33][CH2:32][CH2:31][CH2:30][O:29]4)[C:6]=3[N:7]=[C:8]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH:22]4[CH2:27][CH2:26][CH2:25][CH2:24][O:23]4)=[CH:17][CH:16]=3)[CH:9]=2)=[O:14])[CH2:52][CH2:51]1)=[O:49])([CH3:46])([CH3:44])[CH3:45]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 46942212tert-Butyl 4,7-diazaspiro[2.5]octane-7-carboxylateHCID 118059371HCID 118059371, 화합물

생성물 1

HCID 118059329HCID 118059329, 화합물수율 67.9%

시약·촉매·용매 2

HCID 962Water용매
HCID 6344
Dichloromethane
용매
2회

실험 절차

To a suspension of 300 mg of 3-methyl-1-(tetrahydro-pyran-2-yl)-6-[4-(tetrahydro-pyran-2-yloxy)-phenyl]-1H-pyrazolo[3,4-b]pyridine-4-carboxylic acid sodium salt in 7.5 ml of DCM were added 0.12 ml of Hünig's base, 376 mg of BEP and 146 mg of 4,7-diaza-spiro[2.5]octane-7-carboxylic acid tert-butyl ester. The reaction was stirred overnight at r.t. For workup it was diluted with water and DCM and the layers were separated. The organic layer was washed with water twice, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography (silica, heptane/EtOAc gradient) to obtain 280 mg (66%) of the title compound.

후처리

  1. customthe layers were separated
  2. washThe organic layer was washed with water twice
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash chromatography (silica, heptane/EtOAc gradient)

출처 및 근거

ORD 기록
ord-5f6a679ab82149ab902413ff5a270a51
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09133181B2

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