Acetaldehyde → 2-((2,6-Dimethylpiperidino)amino)propionitrile

HRID 1646383

反応式

HRID 1646383 の反応式
[C-:1]#[N:2].[Na+].[CH:4](=O)[CH3:5].[NH2:7][N:8]1[CH:13]([CH3:14])[CH2:12][CH2:11][CH2:10][CH:9]1[CH3:15].Cl>O.CO>[CH3:15][CH:9]1[CH2:10][CH2:11][CH2:12][CH:13]([CH3:14])[N:8]1[NH:7][CH:4]([CH3:5])[C:1]#[N:2]

参加物

7

反応物 4

HCID 177AcetaldehydeHCID 313Hydrochloric Acid2 回HCID 8929Sodium CyanideHCID 1234822,6-Dimethyl-1-piperidylamine

生成物 1

HCID 150680752-((2,6-Dimethylpiperidino)amino)propionitrile

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒2 回

実験手順

3.9 9 of sodium cyanide, dissolved in 25 ml of water, and 3.5 g of acetaldehyde, dissolved in 25 ml of methanol, are added dropwise with ice-cooling to a mixture of 7.75 g of 1-amino-2,6-dimethylpiperidine, 50 ml of water and 5.2 ml of concentrated hydrochloric acid. The pH of the solution is adjusted to 7 with hydrochloric acid and the reaction mixture is stirred at room temperature for 2 days. After stripping off the methanol, the mixture is extracted with dichloromethane, and the organic phase is dried with sodium sulphate and concentrated. The residue of 9.2 g of 2-((2,6-dimethylpiperidino)amino)propionitrile which remains is processed further without further purification.

後処理

  1. additionare added dropwise with ice-
  2. extractionthe mixture is extracted with dichloromethane
  3. dry with materialthe organic phase is dried with sodium sulphate
  4. concentrationconcentrated
  5. customThe residue of 9.2 g of 2-((2,6-dimethylpiperidino)amino)propionitrile which remains is processed further without further purification

出典と根拠

ORDレコード
ord-821be36b2fb046c2980f158ae31abae5
出典データセット
uspto-grants-1993_01
特許番号
US05179206

関連ノート

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