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HCID 14772476, 화합물 → N-(1,1-Dimethyl-3-oxo-1,3-dihydroisobenzofuran-4-yl)acetamide

HRID 2352451
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HRID 2352451 반응식
[CH3:1][C:2]([OH:16])([CH3:15])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([NH:9][C:10]([CH3:12])=[O:11])[C:4]=1[CH2:13][OH:14]>C(Cl)(Cl)Cl.[O-2].[O-2].[Mn+4]>[CH3:15][C:2]1([CH3:1])[C:3]2[C:4](=[C:5]([NH:9][C:10]([CH3:12])=[O:11])[CH:6]=[CH:7][CH:8]=2)[C:13](=[O:14])[O:16]1
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참가 물질

4

반응물 1

HCID 14772476HCID 14772476, 화합물

생성물 1

HCID 14772477N-(1,1-Dimethyl-3-oxo-1,3-dihydroisobenzofuran-4-yl)acetamide수율 62.2%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 6212Chloroform용매

실험 절차

To a solution of 7.2 g of α,α-dimethyl-2-hydroxymethyl-3-acetaminobenzyl alcohol in 300 ml of chloroform was added 28 g of activated manganese dioxide and the mixture was allowed to react for 6 hours under refluxing. After the reaction was over, the reaction mixture was left to stand for cooling and filtered on a glass filter having a bed of celite. The residue was washed with 100 ml of chloroform. The filtrate and the washed solution were combined and concentrated to obtain an oily substance. The oily substance was purified by silica gel column chromatography to obtain 4.4 g of 3,3-dimethyl-7-acetaminophthalide in the white crystal form. m.p. 124.1° C.

후처리

  1. customto react for 6 hours
  2. temperatureunder refluxing
  3. waitwas left
  4. temperaturefor cooling
  5. filtrationfiltered on a glass
  6. filtrationfilter
  7. washThe residue was washed with 100 ml of chloroform
  8. concentrationconcentrated
  9. customto obtain an oily substance
  10. customThe oily substance was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-f8cd583e732c487c8b5571c49919e28e
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04877441

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