Sodium Carbonate → Methyl (3-(2-methoxyphenyl)phenyl)acetate

HRID 1757065

反応式

HRID 1757065 の反応式
Br[C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH3:12])=[O:10])[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[Na+].[Na+].[CH3:19][O:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1B(O)O.[Cl-].[Na+].C(OCC)(=O)C>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:19][O:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH3:12])=[O:10])[CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 4

HCID 10340Sodium CarbonateHCID 27339582-Methoxyphenylboronic acidHCID 11746402Methyl 2-(3-bromophenyl)acetateHCID 86643102Sodium chloride ethyl acetate

生成物 1

HCID 10848669Methyl (3-(2-methoxyphenyl)phenyl)acetate収率 121.8%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 1140Toluene溶媒2 回

実験手順

Methyl (3-bromophenyl)acetate (2.06 g, 9.0 mmol), tetrakis(triphenylphosphine)palladium (0)(115 mg), sodium carbonate (2.61 g, 25 mmol in 2 ml water) and toluene (10 ml) were degassed under nitrogen in a 25 ml flask fitted with a reflux condenser. 2-Methoxybenzene boronic acid (1.5 g, 9.87 mmol) in toluene (1 ml) was added and the mixture was heated at reflux overnight, then mixed with 1:1 saturated sodium chloride/ethyl acetate (15 ml). The organic materials were separated, dried (MgSO4), then concentrated under reduced pressure which gave 2.81 g of methyl (3-(2-methoxyphenyl)phenyl)acetate.

後処理

  1. customfitted with a reflux condenser
  2. temperaturethe mixture was heated
  3. temperatureat reflux overnight
  4. customThe organic materials were separated
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure which

出典と根拠

ORDレコード
ord-8d532893c93448bd8ffcb6ccfbc7a72e
出典データセット
uspto-grants-1995_08
特許番号
US05444050

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