Nitrogen → HCID 59784760, 화합물

HRID 470331노트

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HRID 470331 반응식
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]

참가 물질

7

반응물 4

HCID 947NitrogenHCID 10340Sodium CarbonateHCID 59784811HCID 59784811, 화합물HCID 178478477HCID 178478477, 화합물

생성물 1

HCID 59784760HCID 59784760, 화합물

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 218864351,4-Dioxane--water (1/1)용매

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온도
100 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-926afb42ee6645948b223723205ca28a
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629147B2

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