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4-Cyclopropylmethoxy-3-methoxy-2-chloromethyl pyridine hydrochloride → 5-Carbomethoxy-6-methyl-2-[[(4-cyclopropylmethoxy-3-methoxy-2-pyridinyl)methyl]thio]-1H-benzimidazole

HRID 1647156
ノート
印刷プレビュー

反応式

HRID 1647156 の反応式
[C:1]([C:5]1[C:14]([CH3:15])=[CH:13][C:8]2[NH:9][C:10]([SH:12])=[N:11][C:7]=2[CH:6]=1)([O:3][CH3:4])=[O:2].Cl.[CH:17]1([CH2:20][O:21][C:22]2[CH:27]=[CH:26][N:25]=[C:24]([CH2:28]Cl)[C:23]=2[O:30][CH3:31])[CH2:19][CH2:18]1>CO>[C:1]([C:5]1[C:14]([CH3:15])=[CH:13][C:8]2[NH:9][C:10]([S:12][CH2:28][C:24]3[C:23]([O:30][CH3:31])=[C:22]([O:21][CH2:20][CH:17]4[CH2:19][CH2:18]4)[CH:27]=[CH:26][N:25]=3)=[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

4

反応物 2

HCID 199264764-Cyclopropylmethoxy-3-methoxy-2-chloromethyl pyridine hydrochlorideHCID 178497010HCID 178497010、化合物

生成物 1

HCID 199264705-Carbomethoxy-6-methyl-2-[[(4-cyclopropylmethoxy-3-methoxy-2-pyridinyl)methyl]thio]-1H-benzimidazole収率 100.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of 5-carbomethoxy-6-methyl-2-mercapto-1H-benzimidazole (0.58 g, 2.6 mmol) in methanol (25 ml) aqueous NaOH (1.0 ml 5M, 5.0 mmol) and 4-cyclopropylmethoxy-3-methoxy-2-chloromethyl pyridine hydrochloride (prepared according to processes known per se.) (0.63 g, 2.4 mmol) dissolved in methanol (25 ml were added in the given order. The mixture was refluxed for one hour whereupon the solution was evaporated. The residue was partitioned between methylene chloride and water. After separation the organic solution was dried over Na2SO4 and evaporated giving a yellow syrup (1.0 g, 100%).

後処理

  1. additionwere added in the given order
  2. temperatureThe mixture was refluxed for one hour whereupon the solution
  3. customwas evaporated
  4. customThe residue was partitioned between methylene chloride and water
  5. customAfter separation the organic solution
  6. dry with materialwas dried over Na2SO4
  7. customevaporated

出典と根拠

ORDレコード
ord-340f439e204b4d43b5533e3fc06000dc
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

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