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3,4-Ethylendioxy-2-chloromethyl pyridine hydrochloride → 5-Acetyl-6-methyl-2-[[(3,4-ethylendioxy-2-pyridinyl)methyl]thio]-1H-benzimidazole

HRID 1647157
ノート
印刷プレビュー

反応式

HRID 1647157 の反応式
[C:1]([C:4]1[C:13]([CH3:14])=[CH:12][C:7]2[NH:8][C:9]([SH:11])=[N:10][C:6]=2[CH:5]=1)(=[O:3])[CH3:2].Cl.[CH2:16]1[CH2:25][O:24][C:23]2[CH:22]=[CH:21][N:20]=[C:19]([CH2:26]Cl)[C:18]=2[O:17]1>CO>[C:1]([C:4]1[C:13]([CH3:14])=[CH:12][C:7]2[NH:8][C:9]([S:11][CH2:26][C:19]3[C:18]4[O:17][CH2:16][CH2:25][O:24][C:23]=4[CH:22]=[CH:21][N:20]=3)=[N:10][C:6]=2[CH:5]=1)(=[O:3])[CH3:2]
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 199264673,4-Ethylendioxy-2-chloromethyl pyridine hydrochlorideHCID 178465846HCID 178465846、化合物

生成物 1

HCID 199264785-Acetyl-6-methyl-2-[[(3,4-ethylendioxy-2-pyridinyl)methyl]thio]-1H-benzimidazole収率 81%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of 5-acetyl-6-methyl-2-mercapto-1H-benzimidazole (0.14 g, 0.66 mmol) in methanol (2 ml) aqueous NaOH (0.25 ml 5M, 1.25 mmol) and 3,4-ethylendioxy-2-chloromethyl pyridine hydrochloride (0.13 g, 0.60 mmol) dissolved in methanol (2 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 (0.17 g, 81%).

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-c161501b4146477ead15e7ae679d2c7d
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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