Piperazine → 2-Piperazin-1-yl-quinazoline

HRID 2270427노트

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HRID 2270427 반응식
Cl[C:2]1[N:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>C1(C)C=CC=CC=1>[N:12]1([C:2]2[N:11]=[CH:10][C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=2)[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 740542-Chloroquinazoline

생성물 1

HCID 64232662-Piperazin-1-yl-quinazoline

시약·촉매·용매 1

HCID 1140Toluene용매2회

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온도
0 °C

실험 절차

A solution of 2-chloroquinazoline (5 g) in 20 mL of toluene is added dropwise to a refluxing solution of piperazine (20 g) in 150 mL of toluene and the resultant solution refluxed for an additional 24 h. After cooling to 0° C. for 0.5 h, the solution is filtered and the filtrate extracted with 10% acetic acid The aqueous extracts are washed with ether, basified and extracted with toluene. The toluene layer is then washed with water, dried and concentrated. Finally, the material is placed under vacuum overnight (6.8, m.p. 188-121° C.).

후처리

  1. filtrationthe solution is filtered
  2. extractionthe filtrate extracted with 10% acetic acid The aqueous extracts
  3. washare washed with ether
  4. extractionextracted with toluene
  5. washThe toluene layer is then washed with water
  6. customdried
  7. concentrationconcentrated
  8. customis placed under vacuum overnight (6.8, m.p. 188-121° C.)

출처 및 근거

ORD 기록
ord-930fd00cfead4ab1aec13f643a7fd316
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06331629B1

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