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Water → Methyl 5-bromo-2-ethylbenzoate

HRID 1625815
ノート
印刷プレビュー

反応式

HRID 1625815 の反応式
[CH2:1]([C:3]1[CH:12]=[CH:11][CH:10]=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6])[CH3:2].[Br:13]Br.C(=O)([O-])[O-].[K+].[K+].O>CO>[Br:13][C:10]1[CH:11]=[CH:12][C:3]([CH2:1][CH3:2])=[C:4]([CH:9]=1)[C:5]([O:7][CH3:8])=[O:6]
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 962WaterHCID 11430Potassium CarbonateHCID 24408BromineHCID 583295Methyl 2-ethylbenzoate

生成物 1

HCID 44226584Methyl 5-bromo-2-ethylbenzoate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The above methyl 2-ethylbenzoate was mixed with molecular sieve 13× (powder, 70 g), and while stirring the mixture, bromine (5.2 ml) was added dropwise thereto at 80° C. The mixture was further stirred at the same temperature for 1.5 hours. The mixture was cooled to room temperature, and added thereto were potassium carbonate (7.4 g), water (70 ml) and methanol (350 ml), and the mixture was stirred for 8 hours. Insoluble materials were filtered off, and suspended in a mixed solution of methanol (500 ml)-water (500 ml), and the mixture was stirred at room temperature overnight. Insoluble materials were filtered off and the filtrate was combined with the previously obtained filtrate, and the solvent was evaporated under reduced pressure. The residue was extracted with ethyl acetate, and the extract was washed with brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was distilled under reduced pressure, to give methyl 5-bromo-2-ethylbenzoate (2.44 g). APCI-Mass m/Z 260/262 (M+NH4).

後処理

  1. additionwas added dropwise
  2. customat 80° C
  3. additionadded
  4. stirringthe mixture was stirred for 8 hours
  5. filtrationInsoluble materials were filtered off
  6. stirringthe mixture was stirred at room temperature overnight
  7. filtrationInsoluble materials were filtered off
  8. customthe solvent was evaporated under reduced pressure
  9. extractionThe residue was extracted with ethyl acetate
  10. washthe extract was washed with brine
  11. dry with materialdried over sodium sulfate
  12. customThe solvent was evaporated under reduced pressure
  13. distillationthe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-5298ee4340694589aa50a170c4ea29cc
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785403B2

反応ノート

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