二甲基对苯二胺二盐酸 → (+-)-2-Amino-2-ethylhex-4-en-1-ol

HRID 850

反应方程式

HRID 850 反应方程式
[NH2:1][C:2]([CH2:12][CH3:13])([CH2:8][CH:9]=[CH:10][CH3:11])[C:3](OCC)=[O:4].[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>C1COCC1>[NH2:1][C:2]([CH2:12][CH3:13])([CH2:8][CH:9]=[CH:10][CH3:11])[CH2:3][OH:4]

参与物

5

反应物 3

HCID 14798二甲基对苯二胺二盐酸HCID 21226445Aluminium lithium hydrideHCID 54508860(+-)-Ethyl 2-amino-2-ethylhex-4-enoate

产物 1

HCID 54018667(+-)-2-Amino-2-ethylhex-4-en-1-ol收率 32.5%

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂2 次

实验过程

A solution of the product from step (d) (116.7 g) in THF (100 ml) was added to a 1M solution of lithium aluminium hydride in THF (800 ml) at about 0° C. When addition was complete, the mixture was stirred overnight at room temperature, then 50% w/v aqu. NaOH (200 ml) was added. The organic phase was separated, washed with brine, dried and evaporated in vacuo. The residue was distilled to give the desired product as an oil (29.3 g). 1H NMR consistent with the proposed structure.

后处理

  1. additionWhen addition
  2. customThe organic phase was separated
  3. washwashed with brine
  4. customdried
  5. customevaporated in vacuo
  6. distillationThe residue was distilled

来源与证据

ORD记录
ord-8bc8a5b260b5493c8773ed6d142bea7c
来源数据集
uspto-grants-1998_03
专利号
US05723458

关联笔记

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