Sulfuric acid magnesium salt (1:1) → HCID 178484438、化合物

HRID 907912ノート

反応式

HRID 907912 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][O:5][C:6]2=[O:11].[CH:12]([C:14]1[CH:24]=[CH:23][C:17]([C:18]([N:20]([CH3:22])[CH3:21])=[O:19])=[CH:16][CH:15]=1)=O.[O-]S([O-])(=O)=O.[Mg+2]>C(#N)C>[CH3:22][N:20]([CH3:21])[C:18](=[O:19])[C:17]1[CH:23]=[CH:24][C:14](/[CH:12]=[N:1]/[C:2]2[CH:10]=[CH:9][CH:8]=[C:7]3[C:3]=2[CH2:4][O:5][C:6]3=[O:11])=[CH:15][CH:16]=1

参加物

5

反応物 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 105592054-formyl-N,N-dimethylbenzamideHCID 122846494-Amino-1,3-dihydro-2-benzofuran-1-one

生成物 1

HCID 178484438HCID 178484438、化合物収率 80.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

4-Aminoisobenzofuran-1(3H)-one (2.10 g, 14.1 mmol), 4-formyl-N,N-dimethylbenzamide (2.50 g, 14.1 mmol) and dry MgSO4 (9.84 g, 82 mmol) were added to acetonitrile (170 mL) and stirred under reflux overnight. The mixture was filtered, and the solvent was evaporated under reduced pressure and the residue was re-crystallized to obtain 3.5 g of title compound as a pale solid. 1H-NMR (400 MHz, CDCl3) δ (ppm): 3.01 (s, 3H), 3.15 (s, 3H), 5.43 (s, 2H), 7.38-7.40 (d, J=7.6 Hz, 1H), 7.55-7.61 (m, 3H), 7.80-7.82 (d, J=7.6 Hz, 1H), 7.96-7.98 (d, J=8 Hz, 2H), 8.58 (s, 1H); LC-MS (ESI) m/z: 308 (M+1)+.

後処理

  1. temperatureunder reflux overnight
  2. filtrationThe mixture was filtered
  3. customthe solvent was evaporated under reduced pressure
  4. customthe residue was re-crystallized

出典と根拠

ORDレコード
ord-effc6bfd86594db2a1ba3c747ca34a5c
出典データセット
uspto-grants-2011_09
特許番号
US08012976B2

反応ノート

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