Ethylamine → Ethyl-(3,5,5-trimethyl-cyclohex-2-enylidene)-amine

HRID 1250431

반응식

HRID 1250431 반응식
[CH2:1]([NH2:3])[CH3:2].O=[C:5]1[CH2:12][C:9]([CH3:11])([CH3:10])[CH2:8][C:7]([CH3:13])=[CH:6]1.[OH-].[K+]>O.Cl.C(N)C>[CH2:1]([N:3]=[C:5]1[CH2:12][C:9]([CH3:11])([CH3:10])[CH2:8][C:7]([CH3:13])=[CH:6]1)[CH3:2]

참가 물질

6

반응물 3

HCID 6341EthylamineHCID 6544IsophoroneHCID 14797Potassium Hydroxide

생성물 1

HCID 11205971Ethyl-(3,5,5-trimethyl-cyclohex-2-enylidene)-amine수율 95%

시약·촉매·용매 2

HCID 11198Ethylamine hydrochloride촉매HCID 962Water용매

반응 조건

온도
10 °C

실험 절차

Ethylamine (42 ml of a 70% solution in water, 530 mmol) is added slowly to a stirred mixture of isophorone (9.67 g, 70 mmol) and ethylamine hydrochloride (0.29 g, 3.5 mmol) at -7° C. After the addition is complete, the temperature of the mixture is allowed to rise to room temperature, and the mixture is stirred for a further 72 hours. The mixture is subsequently cooled to 10° C., and potassium hydroxide (44.9 g, 800 mmol) is added in portions. After 45 minutes, ice is added and the mixture is stirred. The organic phase is then separated, dried over sodium sulfate and evaporated in vacuo to give the crude product (11.0 g, 95%) as a yellow oil, which is used immediately without further purification in the following step.

후처리

  1. additionAfter the addition
  2. customto rise to room temperature
  3. waitAfter 45 minutes
  4. additionice is added
  5. stirringthe mixture is stirred
  6. customThe organic phase is then separated
  7. dry with materialdried over sodium sulfate
  8. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-8887aaeb7acf41b3b6651a248c950fa4
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06339042B1

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