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Thionyl Chloride → 4-Chloro-6-methoxy-7-nitroquinazoline hydrochloride

HRID 634742
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반응식

HRID 634742 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[N+:13]([O-:15])=[O:14])[N:9]=[CH:8][NH:7][C:6]2=O.S(Cl)([Cl:19])=O>CN(C=O)C>[ClH:19].[Cl:19][C:6]1[C:5]2[C:10](=[CH:11][C:12]([N+:13]([O-:15])=[O:14])=[C:3]([O:2][CH3:1])[CH:4]=2)[N:9]=[CH:8][N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 1354520046-Methoxy-7-nitroquinazolin-4(3H)-one

생성물 1

HCID 212603064-Chloro-6-methoxy-7-nitroquinazoline hydrochloride수율 75%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A suspension of 6-methoxy-7-nitro-3,4-dihydroquinazolin-4-one (8 g, 36 mmol) in thionyl chloride (150 ml) and DMF (0.8 ml) was heated at reflux for 3 hours. Excess thionyl chloride was removed by evaporation and the residue azeotroped with toluene. The resulting solid was triturated with ether, collected by filtration and dried under vacuum to give 4-chloro-6-methoxy-7-nitroquinazoline hydrochloride(7.5 g, 75%).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. customExcess thionyl chloride was removed by evaporation
  4. customthe residue azeotroped with toluene
  5. customThe resulting solid was triturated with ether
  6. filtrationcollected by filtration
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-126788b0e06043449c8eb657bf59c5c6
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06184225B2

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