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Sulfuric Acid → 1-[3-Benzo[1,3]dioxol-5-yl-5-(4-methoxy-benzyloxy)-phenyl]-2-methyl-propan-1-one

HRID 417047
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HRID 417047 반응식
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]3[CH:11]=[C:12]([CH:15]=[C:16]([O:18][CH2:19][C:20]4[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=4)[CH:17]=3)[C:13]#N)=[CH:9][C:4]=2[O:3][CH2:2]1.[CH:28]([Mg]Cl)([CH3:30])[CH3:29].S(=O)(=O)(O)[OH:34]>C1COCC1.C(OCC)C>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]3[CH:11]=[C:12]([C:13](=[O:34])[CH:28]([CH3:30])[CH3:29])[CH:15]=[C:16]([O:18][CH2:19][C:20]4[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=4)[CH:17]=3)=[CH:9][C:4]=2[O:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 594968393-Benzo[1,3]dioxol-5-yl-5-(4-methoxy-benzyloxy)-benzonitrileHCID 178418918HCID 178418918, 화합물

생성물 1

HCID 594968191-[3-Benzo[1,3]dioxol-5-yl-5-(4-methoxy-benzyloxy)-phenyl]-2-methyl-propan-1-one수율 64%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

To a solution of 3-benzo[1,3]dioxol-5-yl-5-(4-methoxy-benzyloxy)-benzonitrile (500 mg) in anhydrous THF (10 mL) were added a solution of isopropylmagnesium chloride (2.1 mL of 2 M solution in diethyl ether) and catalytic amount of cuprous bromide (4 mg). The resulting reaction mixture was refluxed for 2 h. After it was cooled down, 10% sulfuric acid (5 mL) was added and stirring was continued for 30 min at room temperature. Then the reaction mixture was diluted with diethyl ether, washed with water and brine. The organic extract was dried over anhydrous sodium sulfate, concentrated and purified on a silica gel column using ethyl acetate and hexanes to yield 358 mg of the title compound (64% yield). HRMS calcd for C25H24O5 [M+H]+ 405.1697, observed 405.1698.

후처리

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed for 2 h
  3. temperatureAfter it was cooled down
  4. washwashed with water and brine
  5. extractionThe organic extract
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. concentrationconcentrated
  8. custompurified on a silica gel column

출처 및 근거

ORD 기록
ord-5adc976157e041c1b8c8cb03e3034de1
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08088936B2

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