Methanol → Methyl 2-(4-fluoro-3-nitrophenyl)acetate

HRID 48169ノート

反応式

HRID 48169 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].S(=O)(=O)(O)O.[CH3:20]O>>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH3:20])=[O:10])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 111272614-Fluoro-3-nitrophenylacetic acid

生成物 1

HCID 22742120Methyl 2-(4-fluoro-3-nitrophenyl)acetate

実験手順

4-Fluoro-3-nitrophenylacetic acid (31.0 g, 0.156 mol) was added to a mixture of concentrated sulfuric acid (1.6 ml) and methanol (160 ml) and the mixture was stirred for 3 days at room temperature. Most of the solvent was removed in vacuo and the residue was partitioned between diethyl ether and water. The organic phase was washed with saturated aqueous sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate, filtered and the filtrate was evaporated in vacuo to give methyl 4-fluoro-3-nitrophenylacetate (27.2 g) as a yellow oil.

後処理

  1. customMost of the solvent was removed in vacuo
  2. customthe residue was partitioned between diethyl ether and water
  3. washThe organic phase was washed with saturated aqueous sodium bicarbonate solution and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customthe filtrate was evaporated in vacuo

出典と根拠

ORDレコード
ord-cda7c95d3a9d45f4a7273c50490ba941
出典データセット
uspto-grants-2004_03
特許番号
US06703347B2

反応ノート

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