Hydrochloric Acid → 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine

HRID 1938112

反応式

HRID 1938112 の反応式
CO.C([O:6][CH:7]([C:9]1[CH:14]=[CH:13][C:12]([C:15]2[N:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])=[CH:17][N:16]=2)=[CH:11][CH:10]=1)[CH3:8])(=O)C.[OH-].[Na+].Cl>C1(C)C=CC=CC=1.O1CCCC1>[OH:6][CH:7]([C:9]1[CH:10]=[CH:11][C:12]([C:15]2[N:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])=[CH:17][N:16]=2)=[CH:13][CH:14]=1)[CH3:8]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 19694897(-)-(4-(1-Acetoxy-ethyl)phenyl)-5-decyloxypyrimidine

生成物 1

HCID 214682802-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine収率 98.5%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Into 100 ml of methanol and 50 ml of tetrahydrofuran were dissolved 15 g of the (-)-2-{4-(1-acetoxyethyl)phenyl}-5-decyloxypyrimidine obtained in Preparation Example [starting material compound (VI)] 70, and then 50 ml of 20% aqueous sodium hydroxide solution were added thereto, to subject to reaction at 40° to 45° C. for 4 hours. After completion of the reaction, 4N hydrochloric acid was added to the reaction mixture to adjust it to pH 7 to 8, and then 200 ml of toluene were added to effect extraction and separation. After the organic phase was washed with water, the solvent was distilled off under reduced pressure to obtain 13.2 g (yield: 98.5%) of (-)-2-{4-(1-hydroxyethyl)phenyl}-5-decyloxypyrimidine.

後処理

  1. customto subject to reaction at 40° to 45° C. for 4 hours
  2. additionwas added to the reaction mixture
  3. washAfter the organic phase was washed with water
  4. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-297227e609b347969998ac9d55ff14cf
出典データセット
uspto-grants-1997_12
特許番号
US05693251

関連ノート

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