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Toluene → 5-(4-Bromo-2,3-difluorophenyl)pyrazin-2-amine

HRID 1523964
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HRID 1523964 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5](B(O)O)=[C:4]([F:11])[C:3]=1[F:12].Br[C:14]1[N:15]=[CH:16][C:17]([NH2:20])=[N:18][CH:19]=1.C1(C)C=CC=CC=1.C([O-])([O-])=O.[Na+].[Na+]>CCO.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>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:14]2[N:15]=[CH:16][C:17]([NH2:20])=[N:18][CH:19]=2)=[C:4]([F:11])[C:3]=1[F:12]
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참가 물질

7

반응물 4

HCID 1140TolueneHCID 10340Sodium CarbonateHCID 5995392-Amino-5-bromopyrazineHCID 27732924-Bromo-2,3-difluorobenzeneboronic acid

생성물 1

HCID 903145395-(4-Bromo-2,3-difluorophenyl)pyrazin-2-amine수율 33%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 702Ethanol용매

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온도
80 °C

실험 절차

A mixture of (4-bromo-2,3-difluorophenyl)boronic acid (400 mg, 1.69 mmol) and 5-bromopyrazin-2-amine (588 mg, 3.38 mmol was suspended in EtOH (5.6 ml) and toluene (5.7 mL) The resulting mixture was treated with aqueous Na2CO3 (2.0 N, 4.2 mL, 8.45 mmol). The resulting mixture was then sparged with nitrogen through the mixture for 10 min, and then Pd(PPh3)4 (98 mg, 0.085 mmol) was added. The reaction vessel was sealed and heated at 80° Celsius for 17 hours. The reaction mixture was cooled to rt and then partitioned between saturated aqueous NH4Cl and EtOAc. The organic layer was dried over MgSO4 and concentrated to dryness. The residue was suspended in DCM and the solid isolated by filtration to afford the title compound (160 mg, 33%), which was used without further purification. MS (ESI): mass calcd. for C10H6BrF2N3, 284.97; m/z found, 286.0 [M+H]+. 1H NMR (400 MHz, DMSO-d6) δ 8.36 (s, 1H), 8.01 (d, J=1.2, 1H), 7.68-7.56 (m, 2H), 6.87 (s, 2H).

후처리

  1. customThe resulting mixture was then sparged with nitrogen through the mixture for 10 min
  2. customThe reaction vessel was sealed
  3. temperatureThe reaction mixture was cooled to rt
  4. custompartitioned between saturated aqueous NH4Cl and EtOAc
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated to dryness
  7. customthe solid isolated by filtration

출처 및 근거

ORD 기록
ord-c9ff847c0a10429a83780defe80b96f5
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09079866B2

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