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Sulfuric acid magnesium salt (1:1) → HCID 178519072、化合物

HRID 1467667
ノート
印刷プレビュー

反応式

HRID 1467667 の反応式
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][C:6]([CH:7]=O)=[CH:5][CH:4]=1.S([O-])([O-])(=O)=O.[Mg+2].[NH2:19][C:20]1[CH:28]=[CH:27][CH:26]=[C:25]2[C:21]=1[CH2:22][O:23][C:24]2=[O:29]>C(#N)C>[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][C:6](/[CH:7]=[N:19]/[C:20]2[CH:28]=[CH:27][CH:26]=[C:25]3[C:21]=2[CH2:22][O:23][C:24]3=[O:29])=[CH:5][CH:4]=1
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 24083Sulfuric acid magnesium salt (1:1)HCID 679964-(Trifluoromethyl)benzaldehydeHCID 122846494-Amino-1,3-dihydro-2-benzofuran-1-one

生成物 1

HCID 178519072HCID 178519072、化合物収率 68.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a stirred mixture of 4-(trifluoromethyl)benzaldehyde (2.8 g, 16.1 mmol) and anhydrous Magnesium sulfate (16 g, 134 mmol) in anhydrous acetonitrile (200 mL) was added 4-aminoisobenzofuran-1(3H)-one (2 g, 13.4 mmol) at room temperature. After the addition, the mixture was stirred at reflux for overnight. The mixture was filtered and the cake was washed with ethyl acetate (50 mL×3). The filtrate was concentrated to give crude product. The crude product was washed with petroleum ether and re-crystallized from ethyl acetate to give the title compound (2.8 g, yield: 68%). LC-MS (ESI) m/z: 306 (M+1)+.

後処理

  1. additionAfter the addition
  2. temperatureat reflux for overnight
  3. filtrationThe mixture was filtered
  4. washthe cake was washed with ethyl acetate (50 mL×3)
  5. concentrationThe filtrate was concentrated
  6. customto give crude product
  7. washThe crude product was washed with petroleum ether
  8. customre-crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-4b000ab114a342978ce3788c075b206c
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08999987B2

反応ノート

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