盐酸羟胺 → 4-(4-t-Butylcyclohexyl)-3-(4-butylpiperazin-1-yl)benzaldehydeoxime

HRID 32249

反应方程式

HRID 32249 反应方程式
[C:1]([CH:5]1[CH2:10][CH2:9][CH:8]([C:11]2[CH:18]=[CH:17][C:14]([CH:15]=O)=[CH:13][C:12]=2[N:19]2[CH2:24][CH2:23][N:22]([CH2:25][CH2:26][CH2:27][CH3:28])[CH2:21][CH2:20]2)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[Cl-].[OH:30][NH3+:31].C([O-])(=O)C.[Na+].[Cl-].[NH4+]>C(OCC)(=O)C.O.C(O)C>[C:1]([CH:5]1[CH2:10][CH2:9][CH:8]([C:11]2[CH:18]=[CH:17][C:14]([CH:15]=[N:31][OH:30])=[CH:13][C:12]=2[N:19]2[CH2:24][CH2:23][N:22]([CH2:25][CH2:26][CH2:27][CH3:28])[CH2:21][CH2:20]2)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2]

参与物

8

反应物 4

HCID 21645盐酸羟胺HCID 25517氯化铵HCID 517045醋酸钠HCID 231425004-(4-t-Butylcyclohexyl)-3-(4-butylpiperazin-1-yl)benzaldehyde

产物 1

HCID 740205524-(4-t-Butylcyclohexyl)-3-(4-butylpiperazin-1-yl)benzaldehydeoxime收率 105.6%

试剂、催化剂与溶剂 3

HCID 702乙醇溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 8857乙酸乙酯溶剂

实验过程

To a mixture of the crude product of 4-(4-t-butylcyclohexyl)-3-(4-butylpiperazin-1-yl)benzaldehyde produced in Example (101b) (247 mg), hydroxylammonium chloride (134 mg, 1.93 mmol) and ethanol (10 mL) were added sodium acetate (193 mg, 2.35 mmol) and water (1.5 mL), followed by stirring for 2 hours at room temperature. The reaction mixture was poured into ice water, and then ethyl acetate and saturated aqueous solution of ammonium chloride were added and extraction was performed with ethyl acetate. The separated organic layer was washed with brine and then dried over anhydrous sodium sulfate. The desiccant was filtered off, and the filtrate was concentrated under reduced pressure to give 271 mg of a crude product of the title compound as a light yellow solid. This product was directly used without purification for the following reaction.

后处理

  1. extractionextraction
  2. washThe separated organic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationThe desiccant was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure

来源与证据

ORD记录
ord-ec9889d94e2147858c604e0aa01348c5
来源数据集
uspto-grants-2008_09
专利号
US07425554B2

关联笔记

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