海萝胶 → 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine

HRID 274180

反应方程式

HRID 274180 反应方程式
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]

参与物

7

反应物 4

HCID 313海萝胶HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮HCID 14798二甲基对苯二胺二盐酸HCID 19694897(-)-(4-(1-Acetoxy-ethyl)phenyl)-5-decyloxypyrimidine

产物 1

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

试剂、催化剂与溶剂 2

HCID 1140甲苯溶剂HCID 8028四氢呋喃溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-4a53a7e9919e42328dec9c7a8d87cefc
来源数据集
uspto-grants-1995_02
专利号
US05389293

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