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Ethyl Acetate → 1H-Indole, 4-(difluoromethoxy)-2,3-dihydro-

HRID 2278657
ノート
印刷プレビュー

反応式

HRID 2278657 の反応式
[CH3:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][CH:5]=[CH:4][C:3]=1[OH:11].Cl[C:13]([F:18])([F:17])C([O-])=O.[Na+].[C:20](=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CN(C)C=O.O>[F:17][CH:13]([F:18])[O:11][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:2]=1[CH2:1][CH2:20][NH:8]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 795792-Methyl-3-nitrophenolHCID 2734985Sodium chlorodifluoroacetate

生成物 1

HCID 866992831H-Indole, 4-(difluoromethoxy)-2,3-dihydro-

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回
HCID 6228
Dimethylformamide
溶媒
2 回

反応条件

温度
110 °C

実験手順

A solution of 10 g of 2-methyl-3-nitrophenol in 20 ml of N,N-dimethylformamide is added to a mixture of 23.4 g of sodium chlorodifluoroacetate and 22 g of potassium carbonate in 30 ml of N,N-dimethylformamide and 6 ml of water. The reaction mixture is then heated at 110° C. for 3 hours and left to stand for 16 hours, and then treated with a mixture of water and ethyl acetate. The organic phase is washed with 1N sodium hydroxide, water and a saturated sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated under reduced pressure, so as to give the expected product in the form of a brown oil, used as it is in the next step.

後処理

  1. waitleft
  2. washThe organic phase is washed with 1N sodium hydroxide, water
  3. dry with materiala saturated sodium chloride solution, dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-db833892bcb44212b36e7746d38f582b
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133168B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート