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2-[1-(2-Fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-6-iodo-7-methyl-7,9-dihydro-8H-purin-8-one → 2-[1-(2-Fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-7-methyl-8-oxo-8,9-dihydro-7H-purine-6-carbonitrile

HRID 510116
ノート
印刷プレビュー

反応式

HRID 510116 の反応式
[F:1][C:2]1[CH:29]=[CH:28][CH:27]=[CH:26][C:3]=1[CH2:4][N:5]1[C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[C:7]([C:14]2[N:22]=[C:21]3[C:17]([N:18]([CH3:24])[C:19](=[O:23])[NH:20]3)=[C:16](I)[N:15]=2)=[N:6]1.[Cu][C:31]#[N:32]>N1C=CC=CC=1>[F:1][C:2]1[CH:29]=[CH:28][CH:27]=[CH:26][C:3]=1[CH2:4][N:5]1[C:9]2=[N:10][CH:11]=[CH:12][CH:13]=[C:8]2[C:7]([C:14]2[N:22]=[C:21]3[C:17]([N:18]([CH3:24])[C:19](=[O:23])[NH:20]3)=[C:16]([C:31]#[N:32])[N:15]=2)=[N:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 867200522-[1-(2-Fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-6-iodo-7-methyl-7,9-dihydro-8H-purin-8-oneHCID 178418546HCID 178418546、化合物

生成物 1

HCID 569289472-[1-(2-Fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-7-methyl-8-oxo-8,9-dihydro-7H-purine-6-carbonitrile収率 19.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

200 mg (0.399 mmol) of the compound obtained in example 107 in pyridine (3 ml) were admixed with 37 mg (0.419 mmol) of copper(I) cyanide and heated to reflux overnight. After cooling, the reaction mixture was filtered and concentrated, and the residue was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient). 31 mg of the title compound were obtained (18% of theory).

後処理

  1. temperatureheated
  2. temperatureto reflux overnight
  3. temperatureAfter cooling
  4. filtrationthe reaction mixture was filtered
  5. concentrationconcentrated
  6. customthe residue was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient)

出典と根拠

ORDレコード
ord-55e04695b06448b488c25828f6df0ad3
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096592B2

反応ノート

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