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

HRID 436203ノート

反応式

HRID 436203 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

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 (6 ml) 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.

後処理

  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

出典と根拠

ORDレコード
ord-8fd5e7acaddd4e6ebefec70337c9997d
出典データセット
uspto-grants-1977_02
特許番号
US04007170

反応ノート

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