Cyclopropylamine → 4-Chloro-6-cyclopropylamino-2-diethylamino-5-pyrimidinecarbonitrile

HRID 1757903ノート

反応式

HRID 1757903 の反応式
Cl[C:2]1[C:7]([C:8]#[N:9])=[C:6]([Cl:10])[N:5]=[C:4]([N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])[N:3]=1.[CH:16]1([NH2:19])[CH2:18][CH2:17]1>CC(C)=O>[Cl:10][C:6]1[C:7]([C:8]#[N:9])=[C:2]([NH:19][CH:16]2[CH2:18][CH2:17]2)[N:3]=[C:4]([N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])[N:5]=1

参加物

4

反応物 2

HCID 69828CyclopropylamineHCID 205101864,6-Dichloro-2-diethylamino-5-pyrimidinecarbonitrile

生成物 1

HCID 205102034-Chloro-6-cyclopropylamino-2-diethylamino-5-pyrimidinecarbonitrile収率 33.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

To a stirred solution of 6.9 grams of 4,6-dichloro-2-diethylamino-5-pyrimidinecarbonitrile in 80 ml of acetone was added dropwise 3.2 grams of cyclopropylamine in 20 ml of acetone. The reaction mixture stood for 16 hours; then the acetone was removed by evaporation under reduced pressure. The residue was washed with water, and the resultant solid was collected. The solid was washed several times with water, then dried, to give 6.5 grams of crude product; mp, 100°-105°. The crude product was recrystallized from petroleum ether to give 2.5 grams of 4-chloro-6-cyclopropylamino-2-diethylamino-5-pyrimidinecarbonitrile; mp, 120°-122°.

後処理

  1. customthen the acetone was removed by evaporation under reduced pressure
  2. washThe residue was washed with water
  3. customthe resultant solid was collected
  4. washThe solid was washed several times with water
  5. customdried
  6. customto give 6.5 grams of crude product
  7. custommp, 100°-105°
  8. customThe crude product was recrystallized from petroleum ether

出典と根拠

ORDレコード
ord-7fdb85c19e20431db0c5469a7057e31b
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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