Methanol → methyl N-[3-(4-phenyl-1-piperazinyl)propyl]dithiocarbamate

HRID 325906

반응식

HRID 325906 반응식
[OH-].[K+].[C:3]1([N:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][NH2:18])[CH2:11][CH2:10]2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:19](=[S:21])=[S:20].[CH3:22]O>>[C:3]1([N:9]2[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:17][NH:18][C:19](=[S:21])[S:20][CH3:22])[CH2:13][CH2:14]2)[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

참가 물질

5

반응물 4

HCID 887MethanolHCID 6348Carbon DisulfideHCID 14797Potassium HydroxideHCID 2612973-(4-Phenylpiperazin-1-yl)propan-1-amine

생성물 1

HCID 12802957methyl N-[3-(4-phenyl-1-piperazinyl)propyl]dithiocarbamate

실험 절차

To a solution of potassium hydroxide (2.85 g) in methanol (25 ml) was added 3-(4-phenyl-1-piperazinyl)propylamine (11.1 g) and thereto was added carbon disulfide (3.85 g) under ice cooling over a period of 10 minutes. The resulting mixture was stirred for 3 hours under ice cooling. The reaction mixture was evaporated under reduced pressure. The residual oil was dissolved in water (40 ml) and washed with diethyl ether. The washed aqueous layer was ice-cooled and thereto was added methyl iodide (7.2 g) with stirring. The resulting mixture was stirred for 2 hours under ice-cooling and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate and then evaporated to give methyl N-[3-(4-phenyl-1-piperazinyl)propyl]dithiocarbamate (12.9 g), mp 75° to 79° C.

후처리

  1. customThe reaction mixture was evaporated under reduced pressure
  2. dissolutionThe residual oil was dissolved in water (40 ml)
  3. washwashed with diethyl ether
  4. temperaturecooled
  5. additionwas added methyl iodide (7.2 g)
  6. stirringwith stirring
  7. stirringThe resulting mixture was stirred for 2 hours under ice-
  8. temperaturecooling
  9. extractionextracted with ethyl acetate
  10. washThe extract was washed with water
  11. dry with materialdried over magnesium sulfate
  12. customevaporated

출처 및 근거

ORD 기록
ord-47a37082f86147eb8754f6b794732fcd
출처 데이터셋
uspto-grants-1984_04
특허 번호
US04443443

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