Iodoethane → HCID 86699746、化合物

HRID 515178ノート

反応式

HRID 515178 の反応式
[Br:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:5]([C:6]([OH:8])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:20](I)[CH3:21]>CN(C=O)C.O>[CH2:20]([O:7][C:6](=[O:8])[C:5]1[C:9]([CH3:11])=[CH:10][C:2]([Br:1])=[CH:3][C:4]=1[O:12][CH3:13])[CH3:21]

参加物

6

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 454803864-Bromo-2-methoxy-6-methylbenzoic acid

生成物 1

HCID 86699746HCID 86699746、化合物収率 89%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of 4-bromo-2-methoxy-6-methyl-benzoic acid (synthesized according to the methods described in sections a) to d) of example 10) (10.7 g, 43.7 mmol) in DMF (90 ml) are added potassium carbonate (12.1 g, 87.3 mmol) and ethyl iodide (17.5 ml, 218 mmol) and the resulting mixture is stirred at room temperature for 2 h. After completion of reaction the reaction mixture is diluted with water (200 ml) and extracted with ethyl acetate (3×50 ml). The combined organic layers are washed with water (2×30 ml), brine (2×30 ml), dried over sodium sulfate and concentrated in vacuo yielding 4-bromo-2-methoxy-6-methyl-benzoic acid ethyl ester (10.5 g, 39 mmol, 89%).

後処理

  1. customAfter completion of reaction the reaction mixture
  2. extractionextracted with ethyl acetate (3×50 ml)
  3. washThe combined organic layers are washed with water (2×30 ml), brine (2×30 ml)
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3674c076dace4675a5d2b55f58989bb4
出典データセット
uspto-grants-2015_08
特許番号
US09108936B2

反応ノート

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