2,6-Dichloropyridine → 2-Chloro-6-(2-Thienylmethoxy)Pyridine

HRID 55118

反応式

HRID 55118 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][OH:7].[H-].[Na+].[Cl:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13](Cl)[N:12]=1>O1CCCC1>[Cl:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([O:7][CH2:6][C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)[N:12]=1

参加物

5

反応物 3

HCID 169892,6-DichloropyridineHCID 24758Sodium hydrideHCID 694672-Thiophenemethanol

生成物 1

HCID 181869442-Chloro-6-(2-Thienylmethoxy)Pyridine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution containing 2-thiophenemethanol (1.5 g, 0.0135×1.0 mol) and sodium hydride (0.58 g, (ca.60% in mineral oil), 0.0135×1.1 mol) in tetrahydrofuran, 2,6-dichloropyridine (2.0 g, 0.0135 mol) was added and the resultant solution was refluxed for about 2 hours. The reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The obtained organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and thereafter, concentrated and purified on a silica gel column to obtain the end product.

後処理

  1. additionwas added
  2. customThe reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
  3. washThe obtained organic layer was washed with aqueous saturated sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. custompurified on a silica gel column
  7. customto obtain the end product

出典と根拠

ORDレコード
ord-03751012921c4d36a4cff78637b58504
出典データセット
uspto-grants-1997_04
特許番号
US05624942

関連ノート

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