聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 3,4-Dihydro-4,4-dimethyl-1(carboethoxymethyl)-6-acetyl-naphthalene

HRID 1387

反应方程式

HRID 1387 反应方程式
[CH3:1][C:2]1([C:7]2[CH:8]=[C:9]3[C:14](=[CH:15][CH:16]=2)[C:13](O)([CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:12][CH2:11][C:10]3([CH3:25])[CH3:24])OCC[O:3]1.CC1C=CC(S(O)(=O)=O)=CC=1.O>C1C=CC=CC=1>[CH3:24][C:10]1([CH3:25])[C:9]2[C:14](=[CH:15][CH:16]=[C:7]([C:2](=[O:3])[CH3:1])[CH:8]=2)[C:13]([CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:12][CH2:11]1

参与物

5

反应物 3

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 6101对甲苯磺酸HCID 18415063(+/-) 6-(2-Methyl-1,3-dioxolan-2-yl)-1,2,3,4-tetrahydro-4,4-dimethyl-1-hydroxy-1-(carboethoxymethyl)-naphthalene

产物 1

HCID 225715193,4-Dihydro-4,4-dimethyl-1(carboethoxymethyl)-6-acetyl-naphthalene

试剂、催化剂与溶剂 1

HCID 241苯溶剂

实验过程

A solution of (±)6-(2-methyl-1,3-dioxolan-2-yl)-1,2,3,4-tetrahydro-4,4-dimethyl-1-hydroxy-1-(carboethoxymethyl)-naphthlene ((Compound D16, 321 mg, 0.90 mmol) and catalytic amount of TsOH in 20 ml of benzene was refluxed for 12 h. During the reaction the water generated from the reaction was periodically removed by a Dean-Stark trap. The solvent was removed and the residue was purified by column chromatography (silica, ethyl acetate/hexane (1/3)) to give the title compound as an oil (215 mg).

后处理

  1. customwas periodically removed by a Dean-Stark trap
  2. customThe solvent was removed
  3. customthe residue was purified by column chromatography (silica, ethyl acetate/hexane (1/3))

来源与证据

ORD记录
ord-46f36199a03b442ba91746cd3e3add7b
来源数据集
uspto-grants-1998_03
专利号
US05723666

关联笔记

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