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

HRID 417050
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인쇄 미리보기

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HRID 417050 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.[CH2:28]([Mg]Cl)[CH3:29].S(=O)(=O)(O)[OH:33]>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:33])[CH2:28][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
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참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 594968393-Benzo[1,3]dioxol-5-yl-5-(4-methoxy-benzyloxy)-benzonitrileHCID 178461633HCID 178461633, 화합물2회

생성물 1

HCID 594968541-[3-Benzo[1,3]dioxol-5-yl-5-(4-methoxy-benzyloxy)-phenyl]-propan-1-one수율 50%

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 (250 mg) in anhydrous THF (3 mL) were added a solution of ethylmagnesium chloride (517 μL of 2 M solution in diethyl ether) and catalytic amount of cuprous bromide (2 mg). The resulting reaction mixture was refluxed for 1 h and then additional amount of ethylmagnesium chloride (517 μL of 2 M solution in diethyl ether) was added and heating was continued for 30 min. After it was cooled down, 10% sulfuric acid (1.5 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 136 mg of the title compound (50% yield). HRMS calcd for C24H22O5 [M+H]+ 391.1540, observed 391.1541.

후처리

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed for 1 h
  3. temperatureheating
  4. temperatureAfter it was cooled down
  5. waitwas continued for 30 min at room temperature
  6. washwashed with water and brine
  7. extractionThe organic extract
  8. dry with materialwas dried over anhydrous sodium sulfate
  9. concentrationconcentrated
  10. custompurified on a silica gel column

출처 및 근거

ORD 기록
ord-41b618635f6f42ed89d5d64e8022a50f
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08088936B2

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