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

HRID 1646383

반응식

HRID 1646383 반응식
[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]

참가 물질

7

반응물 4

HCID 177AcetaldehydeHCID 313Hydrochloric Acid2회HCID 8929Sodium CyanideHCID 1234822,6-Dimethyl-1-piperidylamine

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-821be36b2fb046c2980f158ae31abae5
출처 데이터셋
uspto-grants-1993_01
특허 번호
US05179206

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