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Acetic Anhydride → HCID 73031688、化合物

HRID 1663299
ノート
印刷プレビュー

反応式

HRID 1663299 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=[N:8][N:9]2[CH2:18][C:17]3[C:12](=[CH:13][CH:14]=[C:15]([C:19]([F:28])([C:24]([F:27])([F:26])[F:25])[C:20]([F:23])([F:22])[F:21])[CH:16]=3)[NH:11][C:10]2=[O:29])[CH:2]=1.[H-].[Na+].[C:32](OC(=O)C)(=[O:34])[CH3:33]>CC(N(C)C)=O>[C:32]([N:11]1[C:12]2[C:17](=[CH:16][C:15]([C:19]([F:28])([C:24]([F:25])([F:26])[F:27])[C:20]([F:22])([F:21])[F:23])=[CH:14][CH:13]=2)[CH2:18][N:9]([N:8]=[CH:7][C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)[C:10]1=[O:29])(=[O:34])[CH3:33]
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 3

HCID 7918Acetic AnhydrideHCID 24758Sodium hydrideHCID 730165883,4-dihydro-3-(3-pyridylmethylideneamino)-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone

生成物 1

HCID 73031688HCID 73031688、化合物収率 93.7%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

In 10 ml of dimethylacetamide was dissolved 0.84 g (1.8 mmol) of 3-(3-pyridylmethylideneamino)-3,4-dihydro-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone, and to the resulting solution was added 0.09 g (2.3 mmol) of sodium hydride (purity: 62.4%). The reaction was carried out at room temperature for 30 minutes, after which 0.25 g (2.4 mmol) of acetic anhydride was added and the reaction was carried out for 4 hours. After completion of the reaction, the reaction solution was poured into ice water and the desired compound was extracted with ethyl acetate (20 ml×3). The extract solution was washed with water and saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated in vacuo. The crude product thus obtained was purified by silica gel column chromatography (ethyl acetate−methanol=10:1) to obtain 0.78 g of the desired compound.

後処理

  1. waitthe reaction was carried out for 4 hours
  2. customAfter completion of the reaction
  3. extractionthe desired compound was extracted with ethyl acetate (20 ml×3)
  4. washThe extract solution was washed with water and saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe crude product thus obtained
  8. customwas purified by silica gel column chromatography (ethyl acetate−methanol=10:1)

出典と根拠

ORDレコード
ord-ec75481853414e9c95bd9ae8da094b36
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08034931B2

反応ノート

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