Ethylamine → 3-Chloro-N-ethyl-5,6-diphenyl-2-pyrazinamine

HRID 1578461노트

반응식

HRID 1578461 반응식
Cl[C:2]1[C:7]([Cl:8])=[N:6][C:5]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[C:4]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:3]=1.[CH2:21]([NH2:23])[CH3:22]>CN(C)C=O.O>[Cl:8][C:7]1[C:2]([NH:23][CH2:21][CH3:22])=[N:3][C:4]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[C:5]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:6]=1

참가 물질

5

반응물 2

HCID 6341EthylamineHCID 2792282,3-dichloro-5,6-diphenylpyrazine

생성물 1

HCID 214548043-Chloro-N-ethyl-5,6-diphenyl-2-pyrazinamine

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매2회

실험 절차

2,3-Dichloro-5,6-diphenylpyrazine (2.00 g, 0.0066 moles), is suspended in dimethylformamide (DMF) (12 ml) and treated with a solution of ethylamine (70% in water) (3.5 ml) in DMF (6ml) and the mixture is warmed at 40°-45°C for 30 minutes then allowed to stand at room temperature for 6 hours. The solution is diluted with water (80 ml) and after standing overnight the solid is filtered off, washed with water and dissolved in hot ethyl alcohol, filtered, concentrated and cooled to yield 1.19 g of greenish-yellow solid. m.p. 115°-122°. This material is recrystallized from an ethyl alcohol-hexane mixture, yield 0.84 g, m.p. 121°-125°. Identity of the product is confirmed by infrared, nuclear magnetic resonance and mass spectra.

후처리

  1. temperaturethe mixture is warmed at 40°-45°C for 30 minutes
  2. waitafter standing overnight
  3. filtrationthe solid is filtered off
  4. washwashed with water
  5. dissolutiondissolved in hot ethyl alcohol
  6. filtrationfiltered
  7. concentrationconcentrated
  8. temperaturecooled

출처 및 근거

ORD 기록
ord-7048da1348384fcfafe718e13d1bd7cd
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03936308

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