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Methanol → HCID 178497357, 화합물

HRID 1796340
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HRID 1796340 반응식
[Cl:1][CH2:2][C:3]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([C:12]([OH:14])=[O:13])=[CH:11][C:5]=2[N:4]=1.S(=O)(=O)(O)O.[CH3:20]O>>[Cl:1][CH2:2][C:3]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([C:12]([O:14][CH3:20])=[O:13])=[CH:11][C:5]=2[N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 178524165HCID 178524165, 화합물

생성물 1

HCID 178497357HCID 178497357, 화합물수율 71%

실험 절차

To 2-(Chloromethyl)-1H-benzimidazole-5-carboxylic acid (4) (0.5 g; 2.4 mmole) suspended in anhydrous methanol (20 ml) was added dropwise Sulfuric acid (0.2 ml). The reaction mixture was maintained at reflux for 16 hours. The solvent was evaporated to give the crude oily product, which was purified by column chromatography (silica, 10% methanol: dichloromethane) to obtain 0.4 g (71% yield) of product 5.

후처리

  1. temperatureThe reaction mixture was maintained
  2. temperatureat reflux for 16 hours
  3. customThe solvent was evaporated
  4. customto give the crude oily product, which
  5. customwas purified by column chromatography (silica, 10% methanol: dichloromethane)

출처 및 근거

ORD 기록
ord-868a4287ec894ad8a8a4bf6d592a44da
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07030150B2

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