Water → HCID 839770、化合物

HRID 1076355ノート

反応式

HRID 1076355 の反応式
Cl[C:2]1[N:11]=[C:10](Cl)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[NH:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1.O>O1CCCC1>[N:13]1([C:2]2[N:11]=[C:10]([N:13]3[CH2:17][CH2:16][CH2:15][CH2:14]3)[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=2)[CH2:17][CH2:16][CH2:15][CH2:14]1

参加物

5

反応物 3

HCID 962WaterHCID 31268PyrrolidineHCID 2528862,4-Dichloroquinazoline

生成物 1

HCID 839770HCID 839770、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Ten grams of 2,4-dichloroquinazoline was added carefully to a solution of 25 ml of pyrrolidine in 200 ml of tetrahydrofuran. The resulting mixture was heated at reflux overnight and then was poured into a mixture of ice and water. The resulting mixture was extracted several times with ether. The ether extracts were combined and washed with water. The ether phase then was dried over anhydrous sodium sulfate. The solvent was removed by distillation and the residue was recrystallized from a 1:1 benzene:hexane mixture to give 10.1 g of 2,4-bispyrrolidinylquinazoline; m.p. 127°-129°. The following analytical data were obtained:

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux overnight
  3. extractionThe resulting mixture was extracted several times with ether
  4. washwashed with water
  5. dry with materialThe ether phase then was dried over anhydrous sodium sulfate
  6. customThe solvent was removed by distillation
  7. customthe residue was recrystallized from a 1:1 benzene

出典と根拠

ORDレコード
ord-a5401a0c98174433a795e85e88baa321
出典データセット
uspto-grants-1976_05
特許番号
US03956495

反応ノート

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