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Methyl formate → 5-Carbomethoxy-6-methyl-2-[[(3,4-dimethoxy-2-pyridinyl)methyl]sulfinyl]-1H-benzimidazole

HRID 1647150
ノート
印刷プレビュー

反応式

HRID 1647150 の反応式
[C:1]([C:5]1[C:25]([CH3:26])=[CH:24][C:8]2[NH:9][C:10]([S:12][CH2:13][C:14]3[C:19]([O:20][CH3:21])=[C:18]([O:22][CH3:23])[CH:17]=[CH:16][N:15]=3)=[N:11][C:7]=2[CH:6]=1)([O:3][CH3:4])=[O:2].C([O-])(O)=[O:28].[Na+].ClC1C=CC=C(C(OO)=O)C=1.[OH-].[Na+].C(OC)=O>C(Cl)Cl.O>[C:1]([C:5]1[C:25]([CH3:26])=[CH:24][C:8]2[NH:9][C:10]([S:12]([CH2:13][C:14]3[C:19]([O:20][CH3:21])=[C:18]([O:22][CH3:23])[CH:17]=[CH:16][N:15]=3)=[O:28])=[N:11][C:7]=2[CH:6]=1)([O:3][CH3:4])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 7865Methyl formateHCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 218515495-Carbomethoxy-6-methyl-2-[[(3,4-dimethoxy-2-pyridinyl)methyl]thio]-1H-benzimidazole

生成物 1

HCID 98651425-Carbomethoxy-6-methyl-2-[[(3,4-dimethoxy-2-pyridinyl)methyl]sulfinyl]-1H-benzimidazole
収率 70%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒3 回

実験手順

5--Carbomethoxy-6-methyl-2-[[(3,4-dimethoxy-2-pyridinyl)methyl]thio]-1H-benzimidazole (1.03 g, 0.00276 mol) was dissolved in CH2Cl2 (30 ml). NaHCO3 (0.46 g, 0.0055 mol) in H2O (10 ml) was added and the mixture was cooled to +2° C. m-chloroperbenzoic acid 69.5% (0.62 g, 0.0025 mol) dissolved in CH2Cl2 (5 ml) was added dropwise under stirring. Stirring was continued at +2° C. for 15 min. After separation the organic layer was extracted with an aqueous 0.2M NaOH solution (3×15 ml, 0.009 mol). After separation the aqueous solutions were combined and neutralized with methyl formate (0.56 ml, 0.009 mol) in the presence of CH2Cl2 (25 ml). After separation the organic layer was dried over Na2SO4 and evaporated under reduced pressure. The residue was crystallized from CH3CN (10 ml) giving the title compound (0.68 g, 70%).

後処理

  1. additionwas added dropwise
  2. stirringStirring
  3. customAfter separation the organic layer
  4. customAfter separation the aqueous solutions
  5. customAfter separation the organic layer
  6. dry with materialwas dried over Na2SO4
  7. customevaporated under reduced pressure
  8. customThe residue was crystallized from CH3CN (10 ml)

出典と根拠

ORDレコード
ord-56cbb2624580496596adb4d261fdd9b4
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05430042

反応ノート

読み込み中…

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