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

HRID 598184
ノート
印刷プレビュー

反応式

HRID 598184 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 1

HCID 136400717HCID 136400717、化合物

生成物 1

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

試薬・触媒・溶媒 3

HCID 23994Zinc触媒2 回HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cc001a87d7ce4ae3b050054372b96f01
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897607B2

反応ノート

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