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

HRID 1084471
ノート
印刷プレビュー

反応式

HRID 1084471 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 14772476HCID 14772476、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dcdbdc042639430eb30ce948f02bab92
出典データセット
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05004816

反応ノート

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