6-Thiophen-3-yl-2-(2-trimethylsilanylethoxymethyl)-4-[1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazol-2-yl]-2H-pyridazin-3-one → 4-(1H-Benzimidazol-2-yl)-6-thiophen-3-yl-2H-pyridazin-3-one

HRID 12285

反応式

HRID 12285 の反応式
[S:1]1[CH:5]=[CH:4][C:3]([C:6]2[CH:7]=[C:8]([C:21]3[N:25](COCC[Si](C)(C)C)[C:24]4[CH:34]=[CH:35][CH:36]=[CH:37][C:23]=4[N:22]=3)[C:9](=[O:20])[N:10](COCC[Si](C)(C)C)[N:11]=2)=[CH:2]1>ClCCl.FC(F)(F)C(O)=O.C(S)(S)C>[NH:25]1[C:24]2[CH:34]=[CH:35][CH:36]=[CH:37][C:23]=2[N:22]=[C:21]1[C:8]1[C:9](=[O:20])[NH:10][N:11]=[C:6]([C:3]2[CH:4]=[CH:5][S:1][CH:2]=2)[CH:7]=1

参加物

5

反応物 1

HCID 686802276-Thiophen-3-yl-2-(2-trimethylsilanylethoxymethyl)-4-[1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazol-2-yl]-2H-pyridazin-3-one

生成物 1

HCID 1359787884-(1H-Benzimidazol-2-yl)-6-thiophen-3-yl-2H-pyridazin-3-one

試薬・触媒・溶媒 3

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒HCID 336451,1-Ethanedithiol溶媒

実験手順

30 mg of 6-thiophen-3-yl-2-(2-trimethylsilanylethoxymethyl)-4-[1-(2-trimethylsilanyl -ethoxymethyl)-1H-benzimidazol-2-yl]-2H-pyridazin-3-one is dissolved in a mixture of dichloromethane (1 ml) and trifluoroacetic acid (1 ml), 18 μl of ethanedithiol are added, and the resulting solution is stirred at room temperature for 18 hours. After the solvent has been distilled off, the crude product is purified by preparative RP-HPLC (0-100% acetonitrile (+0.05% formic acid) in water (+0.05% formic acid)).

後処理

  1. additionare added
  2. distillationAfter the solvent has been distilled off
  3. customthe crude product is purified by preparative RP-HPLC (0-100% acetonitrile (+0.05% formic acid) in water (+0.05% formic acid))

出典と根拠

ORDレコード
ord-a0bb0e36af1c4605afc2d9a01c94eb29
出典データセット
uspto-grants-2010_06
特許番号
US07727989B2

関連ノート

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