1-Chloro-3-iodopropane → 3-[N'-(3-Chloropropyl)-N'-methylamino]-N,N,N-trimethyl-1-propanaminium Iodide

HRID 263168

반응식

HRID 263168 반응식
[Br-].[CH3:2][N+:3]([CH3:10])([CH3:9])[CH2:4][CH2:5][CH2:6][NH:7][CH3:8].[I:11][CH2:12][CH2:13][CH2:14][Cl:15]>C(#N)C>[I-:11].[Cl:15][CH2:14][CH2:13][CH2:12][N:7]([CH2:6][CH2:5][CH2:4][N+:3]([CH3:10])([CH3:9])[CH3:2])[CH3:8]

참가 물질

4

반응물 2

HCID 813631-Chloro-3-iodopropaneHCID 21444211N,N,N-Trimethyl-3-(methylamino)propan-1-aminium bromide

생성물 1

HCID 213163753-[N'-(3-Chloropropyl)-N'-methylamino]-N,N,N-trimethyl-1-propanaminium Iodide

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

To a stirred solution of 216.2 mg. (1 mmole) of N,N,N-trimethyl-[3-(methylamino)]-1-propanaminium bromide in 1.5 ml. of acetonitrile is added a solution of 205 mg. (1 mmole) of 3-iodo-1-chloropropane in 0.5 ml. of acetonitrile. The mixture is stirred at room temperature for 2.0 hours and the insoluble N,N,N-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide is removed by filtration. The filtrate is evaporated and the solid residue obtained is extracted with methylene chloride. The methylene chloride extract is evaporated to give the oily product which is recrystallized from isopropanol-ether to afford 90 mg. (52%) of product; m.p. 93° (dec.); NMR δ: 2.2 (3H, S, --NCH3); 3.46 (9H, S, --N+Me3).

후처리

  1. customthe insoluble N,N,N-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide is removed by filtration
  2. customThe filtrate is evaporated
  3. customthe solid residue obtained
  4. extractionis extracted with methylene chloride
  5. extractionThe methylene chloride extract
  6. customis evaporated
  7. customto give the oily product which
  8. customis recrystallized from isopropanol-ether
  9. customto afford 90 mg

출처 및 근거

ORD 기록
ord-ad4325e0b08e4d0881b74275485294cc
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04156693

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