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Hydrochloric Acid → 2-(2-Methoxyphenoxy)benzoic acid

HRID 730065
ノート
印刷プレビュー

反応式

HRID 730065 の反応式
C(=O)([O-])[O-].[Cs+].[Cs+].Br[C:8]1[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=1[C:10]([OH:12])=[O:11].[CH3:17][O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[OH:25].Cl>C1(C)C=CC=CC=1.CC#N.CC#N.CC#N.CC#N.F[P-](F)(F)(F)(F)F.[Cu+].C(OCC)(=O)C>[CH3:17][O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[O:25][C:8]1[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=1[C:10]([OH:12])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 460GuaiacolHCID 69402-Bromobenzoic acidHCID 10796Cesium carbonate

生成物 1

HCID 5786892-(2-Methoxyphenoxy)benzoic acid収率 982.6%

試薬・触媒・溶媒 3

HCID 11068737tetrakis(acetonitrile)copper(I) hexafluorophosphate
触媒
HCID 1140Toluene溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

Tetrakis(acetonitrile)copper(I) hexafluorophosphate (4.62 g, 12.4 mmol), cesium carbonate (32 g, 98 mmol), 2-bromobenzoic acid (10g, 49. 7 mmol) and 2-methoxyphenol (6.17 g, 49.7 mmol) were combined in toluene (100 mL), and the mixture was heated to reflux for 15 hr. Ethyl acetate (200 mL) and 1N HCl (200 mL) were added, and the organic layer was separated. The organic layer was dried over MgSO4, filtered, and evaporated to yield 16.8 g of Compound 1a. The residue was used without further purification. MS m/z (M-H)− 243.1.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 15 hr
  3. customthe organic layer was separated
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-7f2ea80a77f34fedaea6bd83d6e05700
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07582650B2

反応ノート

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