2-氯乙醇 → 2-((3-氟苄基)氨基)乙烷-1-醇

HRID 8638

反应方程式

HRID 8638 反应方程式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][NH2:6].Cl[CH2:11][CH2:12][OH:13].[OH-].[Na+]>O>[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][NH:6][CH2:11][CH2:12][OH:13]

参与物

5

反应物 3

HCID 342-氯乙醇HCID 14798二甲基对苯二胺二盐酸HCID 668533-氟苄胺

产物 1

HCID 108667492-((3-氟苄基)氨基)乙烷-1-醇

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2 次

实验过程

Combine 3-fluorobenzylamine (31.1 g, 0.248 mol), 2-chloroethanol (10 g, 0.124 mol) and water (30 g, 1.66 mol) and heat on a steam-bath for ˜5 hours. Add sodium hydroxide (15 g, 0.373 mol) to the cooled solution and heat the resulting mixture on a steam-bath for ˜30 minutes. Add water (˜50 mL) to dissolve the inorganic salts and extract the two-phase mixture twice with 25 mL and 13 mL portions of benzene. Combine the extracts and remove the water by co-distillation with benzene through a modified Claisen flask. The final desired compound may be purified with further distillation.

后处理

  1. extractionextract the two-phase mixture twice with 25 mL and 13 mL portions of benzene
  2. customremove the water by co-distillation with benzene through a modified Claisen flask
  3. distillationThe final desired compound may be purified with further distillation

来源与证据

ORD记录
ord-96ec3a24686b406a85e6ce4079bf506b
来源数据集
uspto-grants-2006_08
专利号
US07091199B1

关联笔记

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