氢氧化钠 → N,N,N-Trimethyl-3-(methylamino)propan-1-aminium bromide

HRID 263166笔记

反应方程式

HRID 263166 反应方程式
[BrH:1].[Br-].[CH3:3][N+:4]([CH3:11])([CH3:10])[CH2:5][CH2:6][CH2:7][NH:8][CH3:9].[OH-].[Na+]>CO>[Br-:1].[CH3:3][N+:4]([CH3:11])([CH3:10])[CH2:5][CH2:6][CH2:7][NH:8][CH3:9]

参与物

4

反应物 2

HCID 14798氢氧化钠HCID 20320282N,N,N-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide

产物 1

HCID 21444211N,N,N-Trimethyl-3-(methylamino)propan-1-aminium bromide

试剂、催化剂与溶剂 1

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂2 次

实验过程

To a stirred suspension of 876.0 g. (3.0 moles) of N,N,N-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide in 2.75 liters of absolute methanol at room temperature is added a freshly prepared solution of sodium hydroxide (120.0 g., 3.0 moles) in 1.0 liter of absolute methanol over a period of 1.0 hour. The reaction mixture is evaporated under reduced pressure and the solid residue is shaken with 750 ml. of acetonitrile. The insoluble sodium bromide is removed by filtration and the filtrate is evaporated. The solid residue is dried in vacuo to give a quantitative yield of white, crystalline hygroscopic product which may be used without further purification or can be recrystallized from isopropanol-ether. NMR (D2O)δ: 2.28 (3H, S, --NHCH3); 3.11 (9H, S, --N+ (CH3)3).

后处理

  1. additionTo a stirred suspension of 876.0 g
  2. customThe reaction mixture is evaporated under reduced pressure
  3. customThe insoluble sodium bromide is removed by filtration
  4. customthe filtrate is evaporated
  5. customThe solid residue is dried in vacuo
  6. customto give a quantitative yield of white, crystalline hygroscopic product which
  7. custommay be used without further purification
  8. customcan be recrystallized from isopropanol-ether

来源与证据

ORD记录
ord-0662e61bc0864b209a7ae4a35a23a5d4
来源数据集
uspto-grants-1979_05
专利号
US04156693

反应笔记

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