Water → 4-(2-Butynyloxy)-6-phenylpyrimidine

HRID 1759827

反応式

HRID 1759827 の反応式
Cl[C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[CH:4][N:3]=1.[CH2:14]([OH:18])[C:15]#[C:16][CH3:17].[H-].[Na+].O>O1CCCC1>[CH2:14]([O:18][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[CH:4][N:3]=1)[C:15]#[C:16][CH3:17]

参加物

6

反応物 4

HCID 962WaterHCID 129912-Butyn-1-olHCID 24758Sodium hydrideHCID 5934294-Chloro-6-phenylpyrimidine

生成物 1

HCID 225997924-(2-Butynyloxy)-6-phenylpyrimidine収率 86.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In 5 ml of tetrahydrofuran were dissolved 186 mg of 4-chloro-6-phenylpyrimidine and 82 mg of 2-butyn-1-ol, to which 47 mg of sodium hydride (60% in oil) was added with stirring at room temperature, followed by further stirring for 3 hours. The reaction mixture was then poured into water and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated. The resulting residue was subjected to silica gel column chromatography to give 190 mg of 4-(2-butynyloxy)-6-phenylpyrimidine (the present compound (38)), m.p.: 59.6° C.

後処理

  1. stirringby further stirring for 3 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-d88e3aacd89e48dfb367c43646d9e11a
出典データセット
uspto-grants-2005_01
特許番号
US06838463B2

関連ノート

読み込み中…