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Hydrochloric Acid → 4-Iodo-2-phenylquinazoline

HRID 44437
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인쇄 미리보기

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HRID 44437 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:3]=1.Cl.[I-:19].[Na+].C(#N)C>C1COCC1.CCOCC>[I:19][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 6342AcetonitrileHCID 809774-Chloro-2-phenylquinazoline

생성물 1

HCID 159339124-Iodo-2-phenylquinazoline

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

To the 4-chloro-2-phenylquinazoline (4.15 mmol) in dry THF (10 ml) was added a solution of 2 M HCl in ether (4 ml). After 5 min the solvents were removed by vacuum. Dry sodium iodide (41.5 mmol) and acetonitrile (30 ml) were added to the hydrochloride salt and refluxed for 4 hrs. The reaction was quenched by the addition of an aqueous solution of 10% K2CO3 and 5% NaHSO3 (15 ml). Extraction with dichloromethane and drying of the combined organic layers was followed by evaporation of solvents under reduced pressure. The resulting crude product was purified by alumina chromatography with (1:10)

후처리

  1. customAfter 5 min the solvents were removed by vacuum
  2. temperaturerefluxed for 4 hrs
  3. customThe reaction was quenched by the addition of an aqueous solution of 10% K2CO3 and 5% NaHSO3 (15 ml)
  4. extractionExtraction with dichloromethane
  5. customdrying of the combined organic layers
  6. customwas followed by evaporation of solvents under reduced pressure
  7. customThe resulting crude product was purified by alumina chromatography with (1:10)

출처 및 근거

ORD 기록
ord-b9df016134b34f5ba34697fd40377583
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08541428B2

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