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Dimethylformamide → methyl 4-methyl-9-oxo-9H-fluorene-2-carboxylate

HRID 541142
ノート
印刷プレビュー

反応式

HRID 541142 の反応式
[CH3:1][C:2]1[C:14]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:15])[C:6]=2[CH:5]=[C:4]([C:16]([OH:18])=[O:17])[CH:3]=1.[C:19](=O)([O-])[O-].[K+].[K+].CN(C)C=O.CI>O>[CH3:1][C:2]1[C:14]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:15])[C:6]=2[CH:5]=[C:4]([C:16]([O:18][CH3:19])=[O:17])[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 594925644-methyl-9-oxo-9H-fluorene-2-carboxylic acid

生成物 1

HCID 59492531methyl 4-methyl-9-oxo-9H-fluorene-2-carboxylate収率 96.2%

試薬・触媒・溶媒 1

HCID 962Water
溶媒

実験手順

Under anhydrous calcium chloride drying conditions, 4-methyl-9-oxo-9H-fluorene-2-carboxylic acid (1.745 g), potassium carbonate (3.03 g) and dimethylformamide (20 ml) were mixed. To this mixture was added methyl iodide (0.92 ml) at room temperature, and the mixture was stirred for 3 hr 15 min. To the reaction mixture was added water (60 ml), and the mixture was stirred at room temperature for 30 min. The mixture was filtered and the obtained solid was air-dried and dried under reduced pressure at 80° C. to give the title compound (1.778 g, 96%).

後処理

  1. stirringthe mixture was stirred at room temperature for 30 min
  2. filtrationThe mixture was filtered
  3. customthe obtained solid was air-dried
  4. customdried under reduced pressure at 80° C.

出典と根拠

ORDレコード
ord-5c93f162cac6468881f8fa88d7478290
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871934B2

反応ノート

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