Sodium Hydroxide → HCID 47382、化合物

HRID 1439014ノート

反応式

HRID 1439014 の反応式
[CH:1](=[N:3][C:4]([CH2:11][CH2:12][CH3:13])([CH2:8][CH2:9][CH3:10])[CH2:5][CH2:6][CH3:7])[CH3:2].[BH4-].[Na+].[OH-].[Na+]>CO>[CH2:1]([NH:3][C:4]([CH2:11][CH2:12][CH3:13])([CH2:5][CH2:6][CH3:7])[CH2:8][CH2:9][CH3:10])[CH3:2]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 47397N-Ethylidene-4-propyl-4-heptanamineHCID 4311764Sodium borohydride

生成物 1

HCID 47382HCID 47382、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
5 °C

実験手順

Into a 500-ml three-necked flask, fitted with a mechanical stirrer and a condenser, were introduced 17.6 g (0.096 mol) of N-ethylidene-1,1-di-n-propyl-n-butylamine, prepared as described hereabove, and 150 ml of methanol. To this solution when cooled, 7.6 g (0.2 mol) of sodium borohydride were added slowly and while stirring. After this operation, the mixture was maintained at a temperature of 5° C for 30 minutes and then progressively heated under reflux. Thirty minutes later, the methanol was evaporated off under vacuum and 200 ml of water were added to the residue so obtained followed by 100 ml of a solution of sodium hydroxide (d = 1.38). The organic fraction was extracted with ether and the solution was distilled under reduced pressure.

後処理

  1. customInto a 500-ml three-necked flask, fitted with a mechanical stirrer and a condenser
  2. customprepared
  3. temperatureTo this solution when cooled
  4. temperatureprogressively heated
  5. temperatureunder reflux
  6. customThirty minutes later, the methanol was evaporated off under vacuum and 200 ml of water
  7. additionwere added to the residue
  8. customso obtained
  9. extractionThe organic fraction was extracted with ether
  10. distillationthe solution was distilled under reduced pressure

出典と根拠

ORDレコード
ord-901b45e328b74e81bbab48f25b057c2b
出典データセット
uspto-grants-1977_11
特許番号
US04057644

反応ノート

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