Nitrogen → HCID 59784760、化合物

HRID 470331ノート

反応式

HRID 470331 の反応式
NC1C(C(O)=O)=CN(C2N=CC3CC[C:14]4[CH:20]=[C:21]([O:24][CH3:25])C=C[C:13]=4[C:12]=3[N:11]=2)N=1.Br[C:27]1[CH:39]=[CH:38][C:30]2[NH:31]C(C(Cl)(Cl)Cl)=[N:33][C:29]=2[CH:28]=1.C([O-])([O-])=O.[Na+].[Na+].N#N>O1CCOCC1.O.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>[NH2:33][C:29]1[CH:28]=[C:27]([C:20]2[C:21]([O:24][CH3:25])=[N:11][CH:12]=[CH:13][CH:14]=2)[CH:39]=[CH:38][C:30]=1[NH2:31]

参加物

7

反応物 4

HCID 947NitrogenHCID 10340Sodium CarbonateHCID 59784811HCID 59784811、化合物HCID 178478477HCID 178478477、化合物

生成物 1

HCID 59784760HCID 59784760、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 218864351,4-Dioxane--water (1/1)溶媒

反応条件

温度
100 °C

実験手順

To a solution of 4-bromo-o-phenylenediamine 1 (0.935 g, 5 mmol), 2-methoxy-3-pyridyl boronic acid 2 and Na2CO3 (1.060 g, 10 mmols) in 1,4-dioxane/H2O (3:1, 20 mL) flushed with N2 was added Pd(PPh3)4 (0.575 g, 0.5 mmol) in one portion. Resulting reaction mixture was stirred under N2 atmosphere at 100° C. for 12 h. Solvent was evaporated and residue was extracted with ethyl acetate (20 mL). Dried over anhydrous sodiumsulfate. Filtered, and evaporation of solvent gave a crude residue which was used as such in the following reaction. (0.850 g).

後処理

  1. customResulting
  2. customreaction mixture
  3. customSolvent was evaporated
  4. extractionresidue was extracted with ethyl acetate (20 mL)
  5. dry with materialDried over anhydrous sodiumsulfate
  6. filtrationFiltered
  7. customevaporation of solvent

出典と根拠

ORDレコード
ord-926afb42ee6645948b223723205ca28a
出典データセット
uspto-grants-2014_01
特許番号
US08629147B2

反応ノート

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