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HCID 136400717, 화합물 → N-(5-Iodo-7-methyl-4-oxo-4,7-dihydro-3H-pyrrolo[2,3-d]pyrimidin-2-yl)-2,2-dimethylpropanamide

HRID 598184
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HRID 598184 반응식
[I:1][C:2]1[C:10]2[C:9](=[O:11])[NH:8][C:7]([NH:12][C:13](=[O:18])[C:14]([CH3:17])([CH3:16])[CH3:15])=[N:6][C:5]=2[N:4]([CH3:19])[C:3]=1I>C(O)(=O)C.O.[Zn]>[I:1][C:2]1[C:10]2[C:9](=[O:11])[NH:8][C:7]([NH:12][C:13](=[O:18])[C:14]([CH3:15])([CH3:17])[CH3:16])=[N:6][C:5]=2[N:4]([CH3:19])[CH:3]=1
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참가 물질

5

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HCID 136400717HCID 136400717, 화합물

생성물 1

HCID 136400716N-(5-Iodo-7-methyl-4-oxo-4,7-dihydro-3H-pyrrolo[2,3-d]pyrimidin-2-yl)-2,2-dimethylpropanamide수율 78%

시약·촉매·용매 3

HCID 23994Zinc촉매2회HCID 176Acetic Acid용매HCID 962Water용매2회

실험 절차

To a suspension of N-(5,6-diiodo-7-methyl-4-oxo-4,7-dihydro-3H-pyrrolo[2,3-d]pyrimidin-2-yl)-2,2-dimethylpropanamide (941 mg, 1.88 mmol) in acetic acid (9 ml) and water (2 ml) was added zinc powder (246 mg, 3.76 mmol), and the mixture was stirred at room temperature for 1 day. After addition of zinc (123 mg, 1.88 mmol), the mixture was stirred at room temperature for 1 day. The reaction mixture was diluted with water and stirred at 0° C. for 2 hours. The resulting crystals were collected by filtration, washed with water and dissolved in tetrahydrofuran. The solution was filtrated, and the filtrate was concentrated in vacuo. The residue was washed with diiopropyl ether to give 545 mg (78%) of the title compound.

후처리

  1. stirringthe mixture was stirred at room temperature for 1 day
  2. stirringstirred at 0° C. for 2 hours
  3. filtrationThe resulting crystals were collected by filtration
  4. washwashed with water
  5. dissolutiondissolved in tetrahydrofuran
  6. filtrationThe solution was filtrated
  7. concentrationthe filtrate was concentrated in vacuo
  8. washThe residue was washed with diiopropyl ether

출처 및 근거

ORD 기록
ord-cc001a87d7ce4ae3b050054372b96f01
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07897607B2

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