海萝胶 → 苯乙基氨基甲酸甲酯

HRID 1593

反应方程式

HRID 1593 反应方程式
[CH2:1]([NH2:9])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(N(CC)CC)C.Cl[C:18]([O:20][CH3:21])=[O:19].Cl>C1COCC1.C(OCC)C>[CH3:21][O:20][C:18]([NH:9][CH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=[O:19]

参与物

7

反应物 4

HCID 313海萝胶HCID 1001苯乙胺HCID 6586氯甲酸甲酯HCID 8471三乙胺

产物 1

HCID 4380476苯乙基氨基甲酸甲酯收率 95%

试剂、催化剂与溶剂 2

HCID 3283乙醚溶剂HCID 8028四氢呋喃溶剂2 次

实验过程

To a stirred solution of phenethylamine (75.2 mL, 0.6 mol) and triethylamine (83 mL, 0.6 mol) in THF (500 mL) was added slowly methyl chloroformate 46.2 mL, 0.6 mol) dissolved in THF (50 mL). After the reaction was stirred for an additional 1 h at room temperature, diethyl ether (2 L) and 1N HCl (800 mL) were added. The organic layer was washed with water, dried (MgSO4), filtered, and the filtrate was concentrated in vacuo to give a clear oil of pure title compound (102 g, 95%).

后处理

  1. washThe organic layer was washed with water
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated in vacuo

来源与证据

ORD记录
ord-bbd17ea5df144cd0a50c633bd92af129
来源数据集
uspto-grants-1998_03
专利号
US05726159

关联笔记

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