Water → HCID 839770, 화합물

HRID 1076355노트

반응식

HRID 1076355 반응식
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

참가 물질

5

반응물 3

HCID 962WaterHCID 31268PyrrolidineHCID 2528862,4-Dichloroquinazoline

생성물 1

HCID 839770HCID 839770, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-a5401a0c98174433a795e85e88baa321
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03956495

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