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Potassium Phosphate, Tribasic → HCID 68507568、化合物

HRID 1715152
ノート
印刷プレビュー

反応式

HRID 1715152 の反応式
[CH2:1]([O:3][C:4](=[O:15])[C:5]1[CH:10]=[CH:9][C:8](I)=[C:7]([O:12][CH2:13][CH3:14])[CH:6]=1)[CH3:2].[F:16][C:17]1[CH:22]=[CH:21][C:20](B(O)O)=[CH:19][CH:18]=1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>CN(C=O)C.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[CH2:1]([O:3][C:4]([C:5]1[CH:10]=[CH:9][C:8]([C:20]2[CH:21]=[CH:22][C:17]([F:16])=[CH:18][CH:19]=2)=[C:7]([O:12][CH2:13][CH3:14])[CH:6]=1)=[O:15])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 62657Potassium Phosphate, TribasicHCID 2856454-Fluorophenylboronic acidHCID 23090718Ethyl 3-ethoxy-4-iodobenzoate

生成物 1

HCID 68507568HCID 68507568、化合物収率 75%

試薬・触媒・溶媒 2

HCID 11979704Tetrakis(triphenylphosphine)palladium触媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
80 °C

実験手順

To a solution of 3-ethoxy-4-iodo-benzoic acid ethyl ester (0.76 g, 2.37 mmol, 1.0 equiv; [CAS RN 741699-04-7]) in anhydrous DMF (12 mL) under Ar was added 4-fluorophenyl boronic acid (0.40 g, 2.86 mmol, 1.20 equiv), K3PO4 (0.86 g, 4.04 mmol, 1.70 equiv) and tetrakis(triphenylphosphine) palladium(0) (0.082 g, 0.071 mmol, 0.03 equiv) and the reaction mixture heated to 80° C. After 16 h, the reaction mixture was poured on crashed ice/NH4Cl, extracted twice with ethyl acetate, the combined organic phases washed with water and a sat. solution of NaCl, dried over MgSO4 and concentrated by evaporation under reduced pressure. The crude material was purified with silica column chromatography eluting with hexane/ethyl acetate (95:5) to yield 0.51 g (75%) of the title compound as a colorless oil. MS (ISP): 289.3 [M+H]+.

後処理

  1. additionthe reaction mixture was poured
  2. extractionextracted twice with ethyl acetate
  3. washthe combined organic phases washed with water
  4. dry with materiala sat. solution of NaCl, dried over MgSO4
  5. concentrationconcentrated by evaporation under reduced pressure
  6. customThe crude material was purified with silica column chromatography
  7. washeluting with hexane/ethyl acetate (95:5)

出典と根拠

ORDレコード
ord-4ef4acdfdd1d4818ab564ea496c9ba97
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07799806B2

反応ノート

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