聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 2-(4-苯甲氧基苯基)乙醇

HRID 34405

反应方程式

HRID 34405 反应方程式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([O:14][C:15]1[CH:20]=[CH:19][C:18]([CH2:21][C:22](OC)=[O:23])=[CH:17][CH:16]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(OCC)(=O)C.O>CCOCC>[CH2:7]([O:14][C:15]1[CH:16]=[CH:17][C:18]([CH2:21][CH2:22][OH:23])=[CH:19][CH:20]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

参与物

6

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 8857乙酸乙酯HCID 27566454-苯甲氧基苯乙酸甲酯HCID 21226445Aluminium lithium hydride

产物 1

HCID 30172602-(4-苯甲氧基苯基)乙醇

试剂、催化剂与溶剂 1

HCID 3283乙醚溶剂2 次

反应条件

温度
0 °C

实验过程

To a suspension of lithium aluminum hydride (10.8 g, 285 mmoles) in Et2O (300 mL) was very carefully added a solution of methyl 4-(benzyloxy)phenylacetate (6, 72.8 g, 284 mmoles) in Et2O (200 mL) over 40 minutes. After an additional 30 minutes, ethyl acetate (200 mL) was added, followed by H2O (500 mL) and the mixture maintained at 0° C. The mixture was then allowed to separate into two phases. The aqueous phase was extracted with Et2O (2×500 mL). The combined extracts were dried over anhydrous Na2SO4 and evaporated to yield 1-benzyloxy-4-(2-hydroxyethyl)benzene as a white solid, (7, 64.5 g, mp=85° C.). NMR (CDCl3)δppm: 7.33(s, 4H); 6.97(q, 4H); 4.97(s, 2H); 3.67(t, 3H); 4.43(t, 3H); 4.27(s, 1H). (Scheme II, Step 2.)

后处理

  1. customto separate into two phases
  2. extractionThe aqueous phase was extracted with Et2O (2×500 mL)
  3. dry with materialThe combined extracts were dried over anhydrous Na2SO4
  4. customevaporated

来源与证据

ORD记录
ord-f6e7e0fee778474390cb4d0cc375f17e
来源数据集
uspto-grants-1988_08
专利号
US04761420

关联笔记

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