(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 → 4-甲氧基查耳酮

HRID 2101224

反应方程式

HRID 2101224 反应方程式
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[OH-].[Na+].CO.[CH:14](=O)[C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=1>C(OC(=O)C)C>[CH3:22][O:21][C:18]1[CH:19]=[CH:20][C:15]([CH:14]=[CH:2][C:1]([C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)=[O:3])=[CH:16][CH:17]=1

参与物

6

反应物 4

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 7410苯乙酮HCID 14798二甲基对苯二胺二盐酸HCID 31244大茴香醛

产物 1

HCID 941974-甲氧基查耳酮

试剂、催化剂与溶剂 1

HCID 8857乙酸乙酯溶剂

实验过程

Acetophenone (0.5 g) and sodium hydroxide (0.17 g) were suspended in 15 Ml of methanol pre-chilled at −10° C. p-Anisaldehyde (0.57 g) was added thereto, and stirred for 10 hr at room temperature. After neutralization with 5% hydrochloric acid solution, the product was extracted with 100 Ml of ethylacetate. The extracted organic phase was dried with anhydrous magnesium sulfate, and concentrated under vacuum evaporator. Purified compound was obtained by elution with n-hexane:ethylacetate (v/v, 1:7) through silica gel column chromatography (5×3 cm, Merk), and identified as follows:

后处理

  1. additionwas added
  2. extractionAfter neutralization with 5% hydrochloric acid solution, the product was extracted with 100 Ml of ethylacetate
  3. dry with materialThe extracted organic phase was dried with anhydrous magnesium sulfate
  4. concentrationconcentrated under vacuum evaporator
  5. customPurified compound was obtained by elution with n-hexane

来源与证据

ORD记录
ord-6be23af2371049c49a375372ad07cdd3
来源数据集
uspto-grants-2009_08
专利号
US07572831B2

关联笔记

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