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Methyl cyanoacetate → HCID 22097616, 화합물

HRID 1458920
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HRID 1458920 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[NH2:5][C:6]1[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][C:7]=1[C:8]([C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=1)=O.[C:25]([CH2:27][C:28]([O:30][CH3:31])=[O:29])#[N:26]>O>[Cl:24][C:21]1[CH:20]=[C:7]2[C:6](=[CH:23][CH:22]=1)[N:5]=[C:25]([CH2:27][C:28]([O:30][CH3:31])=[O:29])[N:26]=[C:8]2[C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7747Methyl cyanoacetateHCID 6451240Aluminum(III) ChlorideHCID 15592241HCID 15592241, 화합물

생성물 1

HCID 22097616HCID 22097616, 화합물수율 55%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

Powdered aluminium chloride (0.21 g) was added to a mixture of 2-amino-5-chloro-3',4'-dimethoxybenzophenone (0.23 g) and methyl cyanoacetate (5 ml), and the resulting mixture was stirred at 100° C. for 2.5 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over magnesium sulfate, and the solvent was evaporated. The residue was subjected to column chromatography on silica gel. The fractions eluted with hexane/ethyl acetate (4/1, v/v) gave methyl 6-chloro-4-(3,4-dimethoxyphenyl)quinazoline-2-acetate (0.161 g, 55%) which was then recrystallized from isopropyl ether. Colorless needles. mp. 144°-145° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customthe solvent was evaporated
  5. washThe fractions eluted with hexane/ethyl acetate (4/1

출처 및 근거

ORD 기록
ord-06c409ca46b8464f8664064a629a16c0
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05852039

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