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

반응식

HRID 12285 반응식
[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

참가 물질

5

반응물 1

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

생성물 1

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

시약·촉매·용매 3

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매HCID 336451,1-Ethanedithiol용매

실험 절차

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)).

후처리

  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))

출처 및 근거

ORD 기록
ord-a0bb0e36af1c4605afc2d9a01c94eb29
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727989B2

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