Dimethyl Sulfate → HCID 131718384、化合物

HRID 1463825ノート

反応式

HRID 1463825 の反応式
[CH3:1]OS(OC)(=O)=O.[O:8]1[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][NH2:22])[CH2:10][CH2:9]1.[OH-].[Na+]>O>[N:11]1([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][NH:22][CH3:1])[CH2:12][CH2:13][O:8][CH2:9][CH2:10]1

参加物

5

反応物 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 222376608-Morpholinooctylamine

生成物 1

HCID 131718384HCID 131718384、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Dimethylsulphate (832 mg; 0.66 mmoles) was slowly added to 8-morpholinooctylamine (141 mg; 0.66 mmoles) under stirring, the temperature being kept below 70° C. throughout the addition. Stirring was continued overnight. Then the mixture was treated with sodium hydroxide solution (880 mg) in water (15 ml) and heated to boiling. After two hours, the mixture was cooled to room temperature. An oil was separated which was combined with the water layer benzene extracts: the mixture obtained was dried on Na2SO4 and evaporated under reduced pressure. The collected residue was purified by silica gel chromatography, eluting with CHCl3 /MeOH/NH4OH, 65:35:2, to separate the desired product of very intense colour by ninhydrin and iodine reactions.

後処理

  1. additionthe temperature being kept below 70° C. throughout the addition
  2. stirringStirring
  3. temperatureheated to boiling
  4. waitAfter two hours
  5. customAn oil was separated which
  6. customthe mixture obtained
  7. customwas dried on Na2SO4
  8. customevaporated under reduced pressure
  9. customThe collected residue was purified by silica gel chromatography
  10. washeluting with CHCl3 /MeOH/NH4OH, 65:35:2
  11. customto separate the desired product of very intense colour by ninhydrin and iodine reactions

出典と根拠

ORDレコード
ord-ed542e38e8fd4a89ad0b954acdacaedd
出典データセット
uspto-grants-1994_04
特許番号
US05302593

反応ノート

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