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Potassium Phosphate, Tribasic → HCID 68507568、化合物

HRID 1990896
ノート
印刷プレビュー

反応式

HRID 1990896 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], prepared according to WO 04/072 016 A1 (Kissei Pharmaceuticals Co, Ltd.)) in anhydrous DMF (12 mL) under Ar was added 4-fluorophenyl boronic acid (0.40 g, 2.85 mmol, 1.2 equiv), K3PO4 (0.86 g, 4.04 mmol, 1.7 equiv) and tetrakis(triphenylphosphine) palladium(0) (82.3 mg, 0.071 mmol, 0.03 equiv) and the reaction mixture stirred at 80° C. for 16 h. The reaction mixture was poured on ice, extracted with ethyl acetate (2×100 mL) and the combined organic phases washed with water (2×100 mL). The organic phase was dried over MgSO4, concentrated by evaporation under reduced pressure and the crude reaction product purified with column chromatography on silica eluting with hexane/ethyl acetate (95:5) to give 0.51 g (75%) of the title compound.

後処理

  1. additionThe reaction mixture was poured on ice
  2. extractionextracted with ethyl acetate (2×100 mL)
  3. washthe combined organic phases washed with water (2×100 mL)
  4. dry with materialThe organic phase was dried over MgSO4
  5. concentrationconcentrated by evaporation under reduced pressure
  6. customthe crude reaction product
  7. custompurified with column chromatography on silica eluting with hexane/ethyl acetate (95:5)

出典と根拠

ORDレコード
ord-5b2e4a4a60404dafb70e6dd6357b4b51
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07645753B2

反応ノート

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