Dimethyl Ether → HCID 178488689、化合物

HRID 1296945ノート

反応式

HRID 1296945 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:13]([CH3:14])=[N:12][N:11](COCC[Si](C)(C)C)[C:10]=2[C:23]2[CH:24]=[N:25][C:26]([NH2:29])=[N:27][CH:28]=2)=[CH:5][CH:4]=1.B(Cl)(Cl)Cl.COC.C([O-])(O)=O.[Na+]>ClCCl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:13]([CH3:14])=[N:12][NH:11][C:10]=2[C:23]2[CH:28]=[N:27][C:26]([NH2:29])=[N:25][CH:24]=2)=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 8254Dimethyl EtherHCID 25135Boron TrichlorideHCID 516892Sodium BicarbonateHCID 58913495HCID 58913495、化合物

生成物 1

HCID 178488689HCID 178488689、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

5-[4-(4-Methoxy-phenyl)-5-methyl-2-(2-trimethylsilanyl-ethoxymethyl)-2H-pyrazol-3-yl]-pyrimidin-2-ylamine was dissolved in anhydrous dichloromethane under nitrogen. 2M borontrichloride.dimethylether in dichloromethane (7 eq) was added dropwise, and all was stirred for 2 hours. The reaction mixture was added dropwise to sat. NaHCO3(aq) and extracted into dichloromethane. The organic phase was dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by preparative LC/MS to give 5-[4-(4-methoxy-phenyl)-5-methyl-2H-pyrazol-3-yl]-pyrimidin-2-ylamine as a solid.

後処理

  1. extractionextracted into dichloromethane
  2. dry with materialThe organic phase was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by preparative LC/MS

出典と根拠

ORDレコード
ord-455d484964a3435bb8ae951d7731bec7
出典データセット
uspto-grants-2007_07
特許番号
US07247734B2

反応ノート

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