Diethyl Ether → Methyl 2-methoxy-3-nitrobenzoate

HRID 618242ノート

反応式

HRID 618242 の反応式
O[C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7]C=1C(O)=O.IC.[C:16](=[O:19])([O-])[O-].[K+].[K+].C[CH2:23][O:24][CH2:25][CH3:26].CN(C)C=[O:30]>>[CH3:23][O:24][C:25](=[O:30])[C:26]1[CH:7]=[CH:8][CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:2]=1[O:19][CH3:16]

参加物

6

反応物 5

HCID 3283Diethyl EtherHCID 6228DimethylformamideHCID 6328Methyl iodideHCID 68073-Nitrosalicylic acidHCID 11430Potassium Carbonate

生成物 1

HCID 590805Methyl 2-methoxy-3-nitrobenzoate

反応条件

温度
45 °C

実験手順

A solution of 15 g of 2-hydroxy-3-nitro-benzoic acid in 200 ml of N,N-dimethylformamide was treated with 58.1 g of iodomethane and 56.6 g of potassium carbonate, and the resultant heterogeneous mixture was stirred and heated to 45° C. for 20 hr. The mixture was cooled to room temperature, poured into ether, washed with water, washed with saturated sodium carbonate solution, washed with water, dried over magnesium sulfate, evaporated, and 14.2 g of 2-methoxy-3-nitro-benzoic acid methyl ester obtained as an oil which crystallized to a white solid. ##STR135##

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. washwashed with water
  3. washwashed with saturated sodium carbonate solution
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

出典と根拠

ORDレコード
ord-ba6db051f99e446099d47640d714d522
出典データセット
uspto-grants-1999_09
特許番号
US05952362

反応ノート

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