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Acetaldehyde → 2-(Methoxyethylamino)-propionitrile

HRID 745973
ノート
印刷プレビュー

反応式

HRID 745973 の反応式
S(=O)(O)[O-].[Na+].[CH:6](=O)[CH3:7].[CH3:9][O:10][CH2:11][CH2:12][NH2:13].[C-:14]#[N:15].[K+]>O>[CH3:9][O:10][CH2:11][CH2:12][NH:13][CH:6]([CH3:7])[C:14]#[N:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 177AcetaldehydeHCID 80182-MethoxyethylamineHCID 9032Potassium CyanideHCID 23665763Sodium Bisulfite

生成物 1

HCID 137116592-(Methoxyethylamino)-propionitrile収率 87.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred solution of 62.4 g (0.6 mole) sodium bisulfite in 200 ml water which had been cooled in an ice bath, 26.5 g (0.6 mole) acetaldehyde were added over 5 minutes. The ice bath was removed. The reaction mixture was stirred 2.5 hours; then 45 g (0.6 mole) 2-methoxyethylamine were added (with evolution of heat). The reaction mixture was stirred 2 hours; then 39 g (0.6 mole) potassium cyanide were added with heat evolution and the resulting mixture was stirred at ambient temperature. After about 30 minutes, a second phase separated; the reaction mixture was stirred 3 hours and then allowed to stand overnight. The reaction mixture was extracted with 150 ml methylene chloride. The methylene chloride extract was dried over magnesium sulfate and stripped to give 67.4 g of the light yellow oil. The oil was distilled under vacuum to give 60.6 g of the above-identified product as a clear, colorless oil, boiling at 60° C. at 0.20 mm.

後処理

  1. customThe ice bath was removed
  2. temperature(with evolution of heat)
  3. stirringThe reaction mixture was stirred 2 hours
  4. temperaturewith heat evolution
  5. stirringthe resulting mixture was stirred at ambient temperature
  6. waitAfter about 30 minutes
  7. customa second phase separated
  8. stirringthe reaction mixture was stirred 3 hours
  9. waitto stand overnight
  10. extractionThe reaction mixture was extracted with 150 ml methylene chloride
  11. extractionThe methylene chloride extract
  12. dry with materialwas dried over magnesium sulfate

出典と根拠

ORDレコード
ord-b64669c3254647e2b43dad9de6faae2c
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04602029

反応ノート

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