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Potassium Phosphate, Tribasic → HCID 10065775、化合物

HRID 891937
ノート
印刷プレビュー

反応式

HRID 891937 の反応式
[O-]P([O-])([O-])=O.[K+].[K+].[K+].[CH:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH2:12][CH2:11][C:10]=1B(O)O.[Cl:22][C:23]1[CH:24]=[C:25]([CH2:29][N:30]2[CH:34]=[CH:33][N:32]=[C:31]2[CH3:35])[N:26]=[N:27][CH:28]=1.Cl.CCOCC>C1(C)C=CC=CC=1.CO.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1(C2C=CC=CC=2)C=CC=CC=1P(C1CCCCC1)C1CCCCC1>[ClH:22].[CH:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH2:12][CH2:11][C:10]=1[C:23]1[CH:24]=[C:25]([CH2:29][N:30]2[CH:34]=[CH:33][N:32]=[C:31]2[CH3:35])[N:26]=[N:27][CH:28]=1
参加物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 10953452Ether hydrochlorideHCID 117890255-Chloro-3-(2-methylimidazol-1-ylmethyl)-pyridazineHCID 221764573,4-Dihydronaphthalen-2-ylboronic acid2 回

生成物 1

HCID 10065775HCID 10065775、化合物収率 60.3%

試薬・触媒・溶媒 4

HCID 2734216
2-(Dicyclohexylphosphino)biphenyl
触媒
2 回
HCID 178418397HCID 178418397、化合物触媒2 回
HCID 887Methanol溶媒
HCID 1140Toluene溶媒

実験手順

Tetrakis(triphenylphosphine)palladium (0.02 g, 0.017 mmol), biphenyl-2-yl-dicyclohexyl-phosphane (0.005 g, 0.014 mmol), K3PO4 (0.21 g, 1 mmol) and 3,4-dihydro-naphthalene-2-boronic acid (0.13 g, 0.7 mmol) were mixed in degassed toluene (2 ml). 5-Chloro-3-(2-methyl-imidazol-1-yl-methyl)-pyridazine (0.1 g, 0.48 mmol) was added and the mixture was refluxed for 24 hours. After further addition of tetrakis(triphenylphosphine)palladium (0.02 g, 0.017 mmol), biphenyl-2-yl-dicyclohexyl-phosphane (0.005 g, 0.014 mmol) and 3,4-dihydro-naphthalene-2-boronic acid (0.13 g, 0.7 mmol) reflux was continued for another 12 hours. After removal of the solvent in vacuo the residue was dissolved in AcOEt, washed with H2O, dried (Na2SO4) and concentrated in vacuo. The residue was chromatographed over silica gel [gradient CH2Cl2 to 40% (CH2Cl2—MeOH—NH4OH 90:10:1)] to provide a white foam which was dissolved in MeOH (2 ml). HCl-Et2O was added to provide the title compound (0.098 g, 40%) as a light yellow solid, MS: m/e=303.3 (M+).

後処理

  1. temperaturethe mixture was refluxed for 24 hours
  2. temperaturereflux
  3. customAfter removal of the solvent in vacuo the residue
  4. dissolutionwas dissolved in AcOEt
  5. washwashed with H2O
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated in vacuo
  8. customThe residue was chromatographed over silica gel [gradient CH2Cl2 to 40% (CH2Cl2—MeOH—NH4OH 90:10:1)]
  9. customto provide a white foam which

出典と根拠

ORDレコード
ord-648c5b2f3e2a4169beab2907a5f2a38b
出典データセット
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07005432B2

反応ノート

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