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Acetic Anhydride → HCID 58031721、化合物

HRID 40481
ノート
印刷プレビュー

反応式

HRID 40481 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:11]=[CH:10][C:9]2[C:5](=[CH:6][C:7](=[O:12])[N:8]=2)[CH:4]=1.[C:15](OC(=O)C)(=[O:17])[CH3:16]>C1(C)C(C)=CC=CC=1.C(OCC)(=O)C>[C:15]([N:8]1[C:9]2[C:5](=[CH:4][C:3]([C:2]([F:1])([F:13])[F:14])=[CH:11][CH:10]=2)[CH2:6][C:7]1=[O:12])(=[O:17])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 467398615-Trifluoromethyloxoindole

生成物 1

HCID 58031721HCID 58031721、化合物

試薬・触媒・溶媒 2

HCID 7237O-Xylene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2.0 g of 5-trifluoromethyloxoindole were dissolved in 25 ml of xylene, 2.41 ml of acetic anhydride were added and the mixture was heated to boiling under reflux for 5 hours. The reaction solution was cooled to room temperature and diluted with 150 ml of ethyl acetate, and washed with 80 ml each of water, saturated sodium bicarbonate solution and saturated NaCl solution. The organic phase was dried over MgSO4 and concentrated under reduced pressure. The residue was purified on silica gel with the eluent n-heptane=>n-heptane/ethyl acetate=3:1. This gave 1.74 g of 1-acetyl-5-trifluoromethyl-1,3-dihydroindol-2-one as a colorless solid.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. washwashed with 80 ml each of water, saturated sodium bicarbonate solution and saturated NaCl solution
  4. dry with materialThe organic phase was dried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified on silica gel with the eluent n-heptane=>n-heptane/ethyl acetate=3:1

出典と根拠

ORDレコード
ord-2e33e3dec69a4be8869a3b0ce689dbfe
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08530413B2

反応ノート

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