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

HRID 1938112

반응식

HRID 1938112 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-297227e609b347969998ac9d55ff14cf
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05693251

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