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HCID 15036289、化合物 → HCID 15036290、化合物

HRID 728580
ノート
印刷プレビュー

反応式

HRID 728580 の反応式
[CH2:1]([C:3]([OH:18])([CH2:16][CH3:17])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][C:11]([CH3:13])=[O:12])[C:5]=1[CH2:14][OH:15])[CH3:2]>O1CCCC1.[O-2].[O-2].[Mn+4]>[CH2:1]([C:3]1([CH2:16][CH3:17])[C:4]2[C:5](=[C:6]([NH:10][C:11]([CH3:13])=[O:12])[CH:7]=[CH:8][CH:9]=2)[C:14](=[O:15])[O:18]1)[CH3:2]
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 15036289HCID 15036289、化合物

生成物 1

HCID 15036290HCID 15036290、化合物収率 62.2%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 8.0 g of α,α-diethyl-2-hydroxymethyl-3-acetaminobenzyl alcohol in 300 ml of tetrahydrofuran was added 32 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 tetrahydrofuran. 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 4.9 g of 3,3-diethyl-7-acetaminophthalide in the colorless oily substance.

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 tetrahydrofuran
  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-bf1d55aca83741958100901949f36cb8
出典データセット
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05049575

反応ノート

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