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Potassium Phosphate, Tribasic → HCID 58484562、化合物

HRID 1804082
ノート
印刷プレビュー

反応式

HRID 1804082 の反応式
Br[C:2]1[CH:3]=[C:4]([CH3:24])[C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14]([C:16]3[CH:17]=[N:18][C:19]([F:23])=[CH:20][C:21]=3[CH3:22])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].[CH:33]1(B(O)O)[CH2:35][CH2:34]1>O1CCCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1>[CH:33]1([C:2]2[CH:3]=[C:4]([CH3:24])[C:5]([N:8]3[CH2:13][CH2:12][N:11]([C:14]([C:16]4[CH:17]=[N:18][C:19]([F:23])=[CH:20][C:21]=4[CH3:22])=[O:15])[CH2:10][CH2:9]3)=[N:6][CH:7]=2)[CH2:35][CH2:34]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 62657Potassium Phosphate, TribasicHCID 2760897Cyclopropylboronic acidHCID 58484740HCID 58484740、化合物

生成物 1

HCID 58484562HCID 58484562、化合物収率 120.5%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒
HCID 11269872
2-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl
触媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of [4-(5-bromo-3-methylpyridin-2-yl)piperazin-1-yl](6-fluoro-4-methylpyridin-3-yl)methanone (2.2 g) described in Preparation Example 113 in tetrahydrofuran (15 mL) were added 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (229 mg), palladium acetate (125 mg), tripotassium phosphate (3.12 g) and cyclopropylboronic acid (721 mg), and the mixture was refluxed for 7 hr. After cooling, the mixture was extracted with ethyl acetate, washed with saturated brine, and the solvent was evaporated. The residue was purified by column chromatography to give the title compound (2.39 g).

後処理

  1. temperaturethe mixture was refluxed for 7 hr
  2. temperatureAfter cooling
  3. extractionthe mixture was extracted with ethyl acetate
  4. washwashed with saturated brine
  5. customthe solvent was evaporated
  6. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-1d56672ae8d74a62ab55ca743201a53e
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08354401B2

反応ノート

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