Boron trifluoride etherate → 3,4-Difluorophenoxy-3-(4-benzyloxyphenyl)-2-methyl-propionic acid ethyl ester

HRID 348354ノート

反応式

HRID 348354 の反応式
[CH2:1]([O:3][C:4](=[O:32])[C:5]([O:23][C:24]1[CH:29]=[CH:28][C:27]([F:30])=[C:26]([F:31])[CH:25]=1)([CH3:22])[CH:6]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:10][CH:9]=1)O)[CH3:2].B(F)(F)F.CCOCC.C([SiH](CC)CC)C.C([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl>[CH2:1]([O:3][C:4](=[O:32])[C:5]([O:23][C:24]1[CH:29]=[CH:28][C:27]([F:30])=[C:26]([F:31])[CH:25]=1)([CH3:22])[CH2:6][C:8]1[CH:9]=[CH:10][C:11]([O:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:12][CH:13]=1)[CH3:2]

参加物

6

反応物 4

HCID 8000Boron trifluoride etherateHCID 10340Sodium CarbonateHCID 12052TriethylsilaneHCID 693540243-(4-Benzyloxyphenyl)-3-hydroxy-2-(3,4-difluoro-phenoxy)-2-methylpropionic acid ethyl ester

生成物 1

HCID 693538473,4-Difluorophenoxy-3-(4-benzyloxyphenyl)-2-methyl-propionic acid ethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-(4-Benzyloxyphenyl)-3-hydroxy-2-(3,4-difluoro-phenoxy)-2-methylpropionic acid ethyl ester (9.5 mmol) in anhydrous CH2Cl2 (30 mL) was cooled to 0° C. and treated with BF3-Et2O (1.16 mL, 9.5 mmol) and triethylsilane (1.51 mL, 9.5 mmol). The mixture was stirred for 2 h and gradually warmed to ambient temperature. Saturated aqueous Na2CO3 (15 mL) was added and the mixture was stared vigorously. The solution was partitioned and the organic layer was washed twice with water and brine, dried over Na2SO4, and concentrated in vacuo to produce 3-(4-benzyloxyphenyl)-2-(3,4-difluorophenoxy)-2-methylpropionic acid ethyl ester as an oil.

後処理

  1. customThe solution was partitioned
  2. washthe organic layer was washed twice with water and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-da7f2d4129e144f28eae92b8d149cd41
出典データセット
uspto-grants-2007_02
特許番号
US07176224B2

反応ノート

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