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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
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HRID 1647157 반응식
[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]
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참가 물질

4

반응물 2

HCID 199264673,4-Ethylendioxy-2-chloromethyl pyridine hydrochlorideHCID 178465846HCID 178465846, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c161501b4146477ead15e7ae679d2c7d
출처 데이터셋
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05430042

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