Diethylamine → 4-Chloro-6-diethylamino-2-isopropylamino-5-pyrimidinecarbonitrile

HRID 1757896ノート

反応式

HRID 1757896 の反応式
Cl[C:2]1[C:7]([C:8]#[N:9])=[C:6]([Cl:10])[N:5]=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[N:3]=1.[CH2:15]([NH:17][CH2:18][CH3:19])[CH3:16]>C(OCC)C>[Cl:10][C:6]1[C:7]([C:8]#[N:9])=[C:2]([N:17]([CH2:18][CH3:19])[CH2:15][CH3:16])[N:3]=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[N:5]=1

参加物

4

反応物 2

HCID 8021DiethylamineHCID 205102654,6-Dichloro-2-isopropylamino-5-pyrimidinecarbonitrile

生成物 1

HCID 205102144-Chloro-6-diethylamino-2-isopropylamino-5-pyrimidinecarbonitrile収率 50.2%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a stirred solution of 4.3 grams of 4,6-dichloro-2-isopropylamino-5-pyrimidinecarbonitrile in 125 ml of diethyl ether was added dropwise 2.6 grams of diethylamine. Upon complete addition, the reaction mixture was stirred at room temperature for 1.5 hours. The reaction mixture was washed with water. The diethyl ether layer was separated and dried over magnesium sulfate. The mixture was filtered, and the filtrate was evaporated under reduced pressure to a residue. The residue was recrystallized from methylcyclohexane to give 2.5 grams of 4-chloro-6-diethylamino-2-isopropylamino-5-pyrimidinecarbonitrile; mp, 74°-76°.

後処理

  1. additionUpon complete addition
  2. washThe reaction mixture was washed with water
  3. customThe diethyl ether layer was separated
  4. dry with materialdried over magnesium sulfate
  5. filtrationThe mixture was filtered
  6. customthe filtrate was evaporated under reduced pressure to a residue
  7. customThe residue was recrystallized from methylcyclohexane

出典と根拠

ORDレコード
ord-8dd785c8eeac45afbd6744b874eb1cc5
出典データセット
uspto-grants-1983_02
特許番号
USRE031136

反応ノート

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