Sodium Hydroxide → N,N,N-Trimethyl-3-(methylamino)propan-1-aminium bromide

HRID 263166노트

반응식

HRID 263166 반응식
[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]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 20320282N,N,N-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-0662e61bc0864b209a7ae4a35a23a5d4
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04156693

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