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Sodium hydride → 7-bromo-4-(1-(5-ethylpyrimidin-2-yl)piperidin-4-yloxy)-5-methyl-5H-pyrrolo[3,2-d]pyrimidine

HRID 532484
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HRID 532484 반응식
[CH2:1]([C:3]1[CH:4]=[N:5][C:6]([N:9]2[CH2:14][CH2:13][CH:12]([OH:15])[CH2:11][CH2:10]2)=[N:7][CH:8]=1)[CH3:2].[H-].[Na+].[Br:18][C:19]1[C:23]2[N:24]=[CH:25][N:26]=[C:27](Cl)[C:22]=2[N:21]([CH3:29])[CH:20]=1>CN(C=O)C>[Br:18][C:19]1[C:23]2[N:24]=[CH:25][N:26]=[C:27]([O:15][CH:12]3[CH2:11][CH2:10][N:9]([C:6]4[N:7]=[CH:8][C:3]([CH2:1][CH3:2])=[CH:4][N:5]=4)[CH2:14][CH2:13]3)[C:22]=2[N:21]([CH3:29])[CH:20]=1
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참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 577083991-(5-Ethylpyrimidin-2-yl)piperidin-4-olHCID 722079627-bromo-4-chloro-5-methyl-5H-pyrrolo[3,2-d]pyrimidine

생성물 1

HCID 682993167-bromo-4-(1-(5-ethylpyrimidin-2-yl)piperidin-4-yloxy)-5-methyl-5H-pyrrolo[3,2-d]pyrimidine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

1-(5-ethylpyrimidin-2-yl)piperidin-4-ol (93 mg) was added to DMF (5 mL), and cooled to 0° C. Then, NaH (27 mg) was added thereto, and stirred for 30 min. 7-bromo-4-chloro-5-methyl-5H-pyrrolo[3,2-d]pyrimidine (100 mg) was added thereto, and stirred at room temperature for 12 hours. The reaction mixture was extracted with ethyl acetate and distilled water, and the organic layer thus obtained was washed with water and a saline solution. Subsequently, the washed organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain the title compound.

후처리

  1. stirringstirred at room temperature for 12 hours
  2. extractionThe reaction mixture was extracted with ethyl acetate
  3. distillationdistilled water
  4. customthe organic layer thus obtained
  5. washwas washed with water
  6. dry with materialSubsequently, the washed organic layer was dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c91c10788d8043fd9ac61cb1650968a8
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08853213B2

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