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Potassium Phosphate, Tribasic → HCID 178469763、化合物

HRID 593702
ノート
印刷プレビュー

反応式

HRID 593702 の反応式
Cl[C:2]1[C:11]2[C:6](=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:8]=[CH:9][CH:10]=2)[C:5](Cl)=[N:4][N:3]=1.CC1(C)C(C)(C)OB([C:27]2[CH:28]=[N:29][CH:30]=[C:31]([CH:37]=2)[C:32]([O:34][CH2:35][CH3:36])=[O:33])O1.[O-:39]P([O-])([O-])=O.[K+].[K+].[K+].F[B-](F)(F)F.C1([PH+](C2CCCCC2)C2CCCCC2)CCCCC1>O1CCOCC1.O.C([O-])=O.[NH4+].C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[OH:39][C:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][C:7]=2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:2]([C:27]2[CH:28]=[N:29][CH:30]=[C:31]([CH:37]=2)[C:32]([O:34][CH2:35][CH3:36])=[O:33])=[N:3][N:4]=1
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

9

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 3816953Ethyl 5-(tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-3-carboxylateHCID 11710396Tricyclohexylphosphonium TetrafluoroborateHCID 904244121,4-Dichloro-5-phenylphthalazine

生成物 1

HCID 178469763HCID 178469763、化合物収率 51.8%

試薬・触媒・溶媒 4

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒
HCID 2723923Ammonium formate溶媒

反応条件

温度
95 °C

実験手順

To a solution of 1,4-dichloro-5-phenylphthalazine (5.00 g, 18.2 mmol) in 1,4-dioxane (50 mL) and water (9 mL) was added ethyl 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)nicotinate (5.32 g, 27.3 mmol), and K3PO4 (7.72 g, 36.3 mmol). The contents were purged with nitrogen for 10 min. Tricyclohexylphosphonium tetrafluoroborate (0.402 g, 1.09 mmol) was added followed by Pd2(dba)3 (0.416 g, 0.454 mmol) and the reaction mixture was heated at 95° C. for 12 h. The reaction mixture was allowed to cool to ambient temperature and diluted with HCOONH4 buffer (pH˜5) solution. The reaction mixture was extracted with EtOAc (3×75 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The residue was triturated with EtOAc to afford ethyl 5-(4-hydroxy-5-phenylphthalazin-1-yl)nicotinate (3.50 g, 44.1%) as an off-white solid which is 85% pure by LC-MS. LCMS (Condition 1): retention time 2.52 min, [M+1]=372.0. 1H NMR (400 MHz, DMSO-d6) δ 1.37 (t, J=7.2 Hz, 3 H), 4.41 (q, J=7.2 Hz, 2 H), 7.33-7.42 (m, 5 H), 7.62-7.65 (m, 2 H), 7.92 (dd, J=7.6 Hz, J=8.0 Hz, 1 H), 8.49 (t, J=2.0 Hz, 1 H), 9.07 (d, J=2.0 Hz, 1 H), 9.25 (d, J=2.0 Hz, 1 H), 12.74 (br s, 1 H).

後処理

  1. customThe contents were purged with nitrogen for 10 min
  2. temperatureto cool to ambient temperature
  3. extractionThe reaction mixture was extracted with EtOAc (3×75 mL)
  4. dry with materialThe combined organic extracts were dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was triturated with EtOAc

出典と根拠

ORDレコード
ord-b159a69123c8400baa6d818e58940d52
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09242966B2

反応ノート

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