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Methanol → HCID 20252227、化合物

HRID 1284621
ノート
印刷プレビュー

反応式

HRID 1284621 の反応式
[OH-].[K+].[CH2:3]([N:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH2:13][CH2:14][NH2:15])[CH2:8][CH2:7]1)[CH:4]=[CH2:5].[C:16](=[S:18])=[S:17].[CH3:19]O>>[CH2:3]([N:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH2:13][CH2:14][NH:15][C:16](=[S:18])[S:17][CH3:19])[CH2:8][CH2:7]1)[CH:4]=[CH2:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 887MethanolHCID 6348Carbon DisulfideHCID 14797Potassium HydroxideHCID 202522303-[4-(Prop-2-EN-1-YL)piperazin-1-YL]propan-1-amine

生成物 1

HCID 20252227HCID 20252227、化合物

実験手順

To a solution of potassium hydroxide (6.3 g) in methanol (40 m) was added 3-(4-allyl-1-piperazinyl)propylamine (18.8 g) and thereto was added carbon disulfide (7.8 g) under ice cooling over a period of 10 minutes. The resulting mixture was stirred for 2 hours under ice cooling. The reaction mixture was evaporated under reduced pressure. The residual oil was dissolved in water and washed with diethyl ether. The washed aqueous layer was ice-cooled and thereto was added methyl iodide (14.6 g) with stirring. The resulting mixture was stirred for 2 hours under ice-cooling. The reaction mixture was extracted with ethyl acetates, the extract was washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate and then evaporated under reduced pressure to give an oil of methyl N-[3-(4-allyl-1-piperazinyl)propyl]dithiocarbamate (17.7 g).

後処理

  1. customThe reaction mixture was evaporated under reduced pressure
  2. dissolutionThe residual oil was dissolved in water
  3. washwashed with diethyl ether
  4. temperaturecooled
  5. additionwas added methyl iodide (14.6 g)
  6. stirringwith stirring
  7. stirringThe resulting mixture was stirred for 2 hours under ice-
  8. temperaturecooling
  9. extractionThe reaction mixture was extracted with ethyl acetates
  10. washthe extract was washed with a saturated aqueous solution of sodium chloride
  11. dry with materialdried over magnesium sulfate
  12. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-4a218b27217f4c6da79bcb4502a0910a
出典データセット
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04563524

反応ノート

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