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2,2’-[(1-甲基亚乙基)二(4,1-亚苯基氧亚甲基)]二环氧乙烷与α-氢-ω-羟基聚(氧-1,2-亚乙基)的聚合物 → 溴代异丁酸乙二醇酯 溴代异丁酸羟乙醇酯

HRID 2094635
笔记
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反应方程式

HRID 2094635 反应方程式
[CH2:1]([OH:4])[CH2:2][OH:3].C(N(CC)CC)C.[Br:12][C:13]([CH3:18])([CH3:17])[C:14](Br)=[O:15].O>O1CCCC1>[Br:12][C:13]([CH3:18])([CH3:17])[C:14]([O:3][CH2:2][CH2:1][OH:4])=[O:15]
参与物实验过程后处理来源与证据反应笔记

参与物

6

反应物 4

HCID 1742,2’-[(1-甲基亚乙基)二(4,1-亚苯基氧亚甲基)]二环氧乙烷与α-氢-ω-羟基聚(氧-1,2-亚乙基)的聚合物HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 8471三乙胺HCID 886852-溴代异丁酰溴

产物 1

HCID 11481256溴代异丁酸乙二醇酯 溴代异丁酸羟乙醇酯收率 85.3%

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂2 次

实验过程

Anhydrous ethylene glycol (301.3 g, 4.85 mol) and triethylamine (28 mL, 200 mmol) were diluted with dry tetrahydrofuran (100 mL). The reaction mixture was cooled in an ice-water bath and a solution of α-bromoisobutyryl bromide (12 mL, 97.1 mmol) in dry tetrahydrofuran (50 mL) was slowly added while stirring. The mixture was stirred in the cooling bath for 1 h and then at room temperature for 16 h. The reaction mixture was then poured into water (800 mL) and extracted with dichloromethane (6×100 mL). The organic fractions were combined, washed with acidic water (pH=4), dried over MgSO4 and evaporated to dryness to afford 17.477 g (yield=85.3%) of a very pale yellow liquid. 1H NMR (CDCl3, δ, ppm): 4.30-4.19 (m, 2H), 3.86-3.75 (m, 2H), 2.86-2.47 (broad peak, 1H, OH), 1.89 (s, 6H). 13C NMR (CDCl3, δ): 171.95, 67.40, 60.63, 55.89, 30.72.

后处理

  1. temperatureThe reaction mixture was cooled in an ice-water bath
  2. stirringThe mixture was stirred in the cooling bath for 1 h
  3. extractionextracted with dichloromethane (6×100 mL)
  4. washwashed with acidic water (pH=4)
  5. dry with materialdried over MgSO4
  6. customevaporated to dryness
  7. customto afford 17.477 g (yield=85.3%) of a very pale yellow liquid

来源与证据

ORD记录
ord-41b8f61f722b45d59749807dd79976b5
来源数据集
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08445610B2

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