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Methanesulfonic Acid → 5-(5-Cyanobenzoxazol-2-yl)-2-methyl-1-(tetrahydropyran-4-yl)benzimidazole

HRID 74247
ノート
印刷プレビュー

反応式

HRID 74247 の反応式
Cl.[CH3:2][C:3]1[N:7]([CH:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[C:6]2[CH:14]=[CH:15][C:16]([C:18]([OH:20])=O)=[CH:17][C:5]=2[N:4]=1.S(Cl)(Cl)=O.[NH2:25][C:26]1[CH:31]=[C:30]([C:32]#[N:33])[CH:29]=[CH:28][C:27]=1O.C(N(CC)CC)C.CS(O)(=O)=O.C(=O)([O-])O.[Na+]>O.O1CCCC1>[C:32]([C:30]1[CH:29]=[CH:28][C:27]2[O:20][C:18]([C:16]3[CH:15]=[CH:14][C:6]4[N:7]([CH:8]5[CH2:9][CH2:10][O:11][CH2:12][CH2:13]5)[C:3]([CH3:2])=[N:4][C:5]=4[CH:17]=3)=[N:25][C:26]=2[CH:31]=1)#[N:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 6395Methanesulfonic AcidHCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 2712583-Amino-4-hydroxybenzonitrileHCID 516892Sodium BicarbonateHCID 674984452-methyl-1-(tetrahydropyran-4-yl)benzimidazole-5-carboxylic acid HCl salt

生成物 1

HCID 67498037
5-(5-Cyanobenzoxazol-2-yl)-2-methyl-1-(tetrahydropyran-4-yl)benzimidazole
収率 12%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To 2-methyl-1-(tetrahydropyran-4-yl)benzimidazole-5-carboxylic acid HCl salt (see Working Example 4-3) (182 mg, 0.612 mmol) was added thionyl chloride (2 mL), and this was stirred at reflux for 3 hours. After the reaction was complete, concentration at reduced pressure gave a residue that was added to 2-amino-4-cyanophenol (82.1 mg, 0.612 mmol), triethylamine (309 mg, 3.06 mmol) and tetrahydrofuran (5 mL), and this was stirred at room temperature for 14 hours. After the reaction was complete, this was concentrated, and to a dioxane (5 mL) solution of the residue obtained was added methanesulfonic acid (353 mg, 1.46 mmol), and this was heated to reflux for 18 hours. After the reaction solution was cooled, water and saturated aqueous sodium hydrogen carbonate solution were added, and this was extracted with chloroform. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. The residue obtained was purified by silica gel column chromatography to yield the title compound (26.1 mg, 12% yield) as pale yellow crystals.

後処理

  1. temperatureat reflux for 3 hours
  2. concentrationconcentration at reduced pressure
  3. customgave a residue that
  4. stirringthis was stirred at room temperature for 14 hours
  5. concentrationthis was concentrated
  6. customto a dioxane (5 mL) solution of the residue obtained
  7. temperaturethis was heated
  8. temperatureto reflux for 18 hours
  9. temperatureAfter the reaction solution was cooled
  10. extractionthis was extracted with chloroform
  11. customAfter the organic layer obtained
  12. dry with materialwas dried over anhydrous sodium sulfate, it
  13. filtrationwas filtered
  14. concentrationconcentrated
  15. customThe residue obtained
  16. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-adf43a9ef3e74fc38d79df2417c9687b
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829035B2

反応ノート

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