Ethanol → 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine

HRID 274176

反応式

HRID 274176 の反応式
C(O)C.C(Cl)(Cl)Cl.[C:8]([C:11]1[CH:16]=[CH:15][C:14]([C:17]2[N:22]=[CH:21][C:20]([O:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33])=[CH:19][N:18]=2)=[CH:13][CH:12]=1)(=[O:10])[CH3:9].[BH4-].[Na+]>O>[OH:10][CH:8]([C:11]1[CH:12]=[CH:13][C:14]([C:17]2[N:22]=[CH:21][C:20]([O:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33])=[CH:19][N:18]=2)=[CH:15][CH:16]=1)[CH3:9]

参加物

6

反応物 4

HCID 702EthanolHCID 6212ChloroformHCID 4311764Sodium borohydrideHCID 196949012-(4-Acetylphenyl)-5-decyloxypyrimidine

生成物 1

HCID 214682802-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine収率 99.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixed solvent of 200 ml of ethanol and 100 ml of chloroform were added 35.5 g (0.1 mole) of 2-(4-acetylphenyl)-5-decyloxypyrimidine, and while maintaining the temperature at 30° to 35° C., 2.65 g (0.07 mole) of sodium borohydride were gradually added thereto. After stirring at the same temperature for 4 hours, the reaction mixture was poured into 500 ml of water and extracted with 400 ml of ethyl acetate. The organic phase was washed sufficiently, dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure to obtain 35.6 g (yield: 99.9%) of 2-{4-(1-hydroxyethyl)phenyl}-5-decyloxypyrimidine.

後処理

  1. temperaturewhile maintaining the temperature at 30° to 35° C.
  2. extractionextracted with 400 ml of ethyl acetate
  3. washThe organic phase was washed sufficiently
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-39cf154310904a01a5566707314467d7
出典データセット
uspto-grants-1995_02
特許番号
US05389293

関連ノート

読み込み中…