Methyl iodide → Benzoic acid, 5-methoxy-2-methyl-3-nitro-, methyl ester

HRID 2208917ノート

反応式

HRID 2208917 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5](C)=[C:6]([CH:10]=1)C(O)=O.[C:15](=O)([O-])[O-].[Na+].[Na+].CI.[C:23]([O:26][CH2:27]C)(=[O:25])[CH3:24]>CN(C=O)C.O>[CH3:15][O:1][C:2]1[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5]([CH3:6])=[C:24]([CH:10]=1)[C:23]([O:26][CH3:27])=[O:25]

参加物

7

反応物 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 10340Sodium CarbonateHCID 23009717HCID 23009717、化合物

生成物 1

HCID 53399479Benzoic acid, 5-methoxy-2-methyl-3-nitro-, methyl ester

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

To a stirred solution of 5-hydroxy-2-methyl-3-nitrobenzoic acid (1.50 g, 7.61 mmol) in DMF (15 mL) was added sodium carbonate (3.23 g, 30.5 mmol) and methyl iodide (1.88 mL, 30.5 mmol). The resulting reaction mixture was heated at 60° C. for 8 h. On completion, the reaction mixture was diluted with water and extraction was carried out using ethyl acetate. The combined organic layers were dried and concentrated under reduced pressure to give the crude title compound (1.7 g) which was used directly in the next step.

後処理

  1. customThe resulting reaction mixture
  2. customThe combined organic layers were dried
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-e5fa4c38e4e94694965a113c9df36cac
出典データセット
uspto-grants-2016_06
特許番号
US09376422B2

反応ノート

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