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吡啶 → (4-Oxo-1-phenylcyclohexyl)methyl acetate

HRID 1576216
笔记
打印预览

反应方程式

HRID 1576216 反应方程式
[OH:1][CH2:2][C:3]1([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.N1C=CC=CC=1.[C:22](OC(=O)C)(=[O:24])[CH3:23]>O>[C:22]([O:1][CH2:2][C:3]1([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH2:4][CH2:5][C:6](=[O:9])[CH2:7][CH2:8]1)(=[O:24])[CH3:23]
参与物实验过程后处理来源与证据反应笔记

参与物

5

反应物 3

HCID 1049吡啶HCID 7918乙酐HCID 215146764-(Hydroxymethyl)-4-phenylcyclohexan-1-one

产物 1

HCID 21514685(4-Oxo-1-phenylcyclohexyl)methyl acetate收率 35.8%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

6.6 g. of 4-hydroxymethyl-4-phenylcyclohexanone is dissolved in 40 ml. of pyridine and 20 ml. acetic anhydride. After about 20 hours of standing at room temperature, the mixture is poured into ice and water. The gum that precipitates is extracted with ether. The organic layer is washed successively with water, 2.5 N hydrochloric acid, water, sodium bicarbonate solution, and brine, and then evaporated to dryness. The solid residue is recrystallized from Skellysolve B to give 6.74 g. (35.8% yield) of 4-acetoxymethyl-4-phenylcyclohexanone, having a melting point of 74° to 79°C.

后处理

  1. customThe gum that precipitates
  2. extractionis extracted with ether
  3. washThe organic layer is washed successively with water, 2.5 N hydrochloric acid, water, sodium bicarbonate solution, and brine
  4. customevaporated to dryness
  5. customThe solid residue is recrystallized from Skellysolve B
  6. customto give 6.74 g

来源与证据

ORD记录
ord-ebf73aacd42445a5a9b53afbcc3f23c5
来源数据集
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
专利号
US03979444

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记