Pyridinium chloride → HCID 68554841, 화합물

HRID 2359883노트

반응식

HRID 2359883 반응식
C[O:2][C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=[C:7]1[NH2:16].Cl.N1C=CC=CC=1>O>[NH2:16][C:7]1[N:6]([CH2:5][C:4]2[CH:17]=[CH:18][CH:19]=[CH:20][C:3]=2[OH:2])[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=1

참가 물질

4

반응물 2

HCID 10176127Pyridinium chlorideHCID 68550921HCID 68550921, 화합물

생성물 1

HCID 68554841HCID 68554841, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
140 °C

실험 절차

120 mg (0.45 mmol) 3-(2-methoxybenzyl)-3,4-dihydroquinazolin-2-amine and 5 g pyridine hydrochloride were combined and heated for 4 hours at approx. 140° C. After cooling the melt, the residue was dissolved in water, extracted three times with dichloromethane and the combined organic phases were dried, filtered and evaporated. The resulting crude product was purified over MPLC (silica gel: Bischoff Prontoprep 60-2540-C18E, 32 μm; mobile phase: CH3CN/H2O+0.1% acetic acid) and subsequent lyophilization yielded the target product as a beige white solid; 110 mg.

후처리

  1. temperatureAfter cooling the melt
  2. extractionextracted three times with dichloromethane
  3. customthe combined organic phases were dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe resulting crude product was purified over MPLC (silica gel: Bischoff Prontoprep 60-2540-C18E, 32 μm; mobile phase: CH3CN/H2O+0.1% acetic acid) and subsequent lyophilization

출처 및 근거

ORD 기록
ord-e27a5b14b6bc467db73f5f03f6a8c3b8
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08686002B2

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