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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Pyridine → 3-(2-bromo-phenyl)-3,4-dihydro-7-[2-(p-toluenesulfonyl)oxymethyl-benzodioxane-6 yl]amino-1-methyl-pyrimido[4,5-d]pyrimidin-2 (1H)-one

HRID 9728
ノート
印刷プレビュー

反応式

HRID 9728 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:17][C:16]2[C:11](=[N:12][C:13]([NH:18][C:19]3[CH:30]=[CH:29][C:22]4[O:23][CH:24]([CH2:27][OH:28])[CH2:25][O:26][C:21]=4[CH:20]=3)=[N:14][CH:15]=2)[N:10]([CH3:31])[C:9]1=[O:32].[S:33](Cl)([C:36]1[CH:42]=[CH:41][C:39]([CH3:40])=[CH:38][CH:37]=1)(=[O:35])=[O:34].N1C=CC=CC=1>C(Cl)(Cl)Cl.CN(C)C1C=CN=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:17][C:16]2[C:11](=[N:12][C:13]([NH:18][C:19]3[CH:30]=[CH:29][C:22]4[O:23][CH:24]([CH2:27][O:28][S:33]([C:36]5[CH:42]=[CH:41][C:39]([CH3:40])=[CH:38][CH:37]=5)(=[O:35])=[O:34])[CH2:25][O:26][C:21]=4[CH:20]=3)=[N:14][CH:15]=2)[N:10]([CH3:31])[C:9]1=[O:32]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 1049PyridineHCID 73974-Toluenesulfonyl chloride2 回HCID 10345790PharmaGSID_48519

生成物 1

HCID 865921593-(2-bromo-phenyl)-3,4-dihydro-7-[2-(p-toluenesulfonyl)oxymethyl-benzodioxane-6 yl]amino-1-methyl-pyrimido[4,5-d]pyrimidin-2 (1H)-one収率 26.4%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine
触媒
HCID 6212Chloroform溶媒2 回

反応条件

温度
5 °C

実験手順

520 mg of the product from example 1 were dissolved in 20 ml CHCl3. 213 mg tosyl chloride and 13 mg 4-dimethylaminopyridine were added and the mixture was cooled to 5° C. 166 mg pyridine were added dropwise and stirring was continued at room temperature for 3 hrs. The mixture was stirred 1 hr at 60° C., then another 105 mg tosyl chloride were added and stirring was continued at room temperature for 16 hrs. The mixture was diluted with 50 ml CHCl3 and washed with 0.5 M HCl, dried and evaporated. Chromatography on silica yielded 180 mg of the title compound.

後処理

  1. stirringThe mixture was stirred 1 hr at 60° C.
  2. stirringstirring
  3. waitwas continued at room temperature for 16 hrs
  4. washwashed with 0.5 M HCl
  5. customdried
  6. customevaporated

出典と根拠

ORDレコード
ord-2f4ba6433b594125bf21b306ef755b52
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07091345B2

反応ノート

読み込み中…

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