Potassium Carbonate → HCID 18446520, 화합물

HRID 1868287노트

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HRID 1868287 반응식
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][NH2:8])=[CH:5][CH:4]=1.C([O-])([O-])=O.[K+].[K+].[Br:17][C:18]1[S:26][C:25]2[C:24]([C:27]#[N:28])=[CH:23][N:22]=[C:21](Cl)[C:20]=2[CH:19]=1>CN1CCCC1=O>[Br:17][C:18]1[S:26][C:25]2[C:24]([C:27]#[N:28])=[CH:23][N:22]=[C:21]([NH:8][CH2:7][C:6]3[CH:9]=[CH:10][C:3]([O:2][CH3:1])=[CH:4][CH:5]=3)[C:20]=2[CH:19]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 754524-MethoxybenzylamineHCID 184465172-Bromo-4-chlorothieno[3,2-c]pyridine-7-carbonitrile

생성물 1

HCID 18446520HCID 18446520, 화합물수율 66.5%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

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온도
130 °C

실험 절차

To a stirred solution of 4-methoxybenzylamine (1.2 equiv., 2.4 mmol) and K2CO3 (2.4 equiv., 4.8 mmol) in 5 mL anhydrous 1-methyl-2-pyrrolidinone was added 15 (1 equiv., 2 mmol). The mixture was heated at 130° C. under N2 for 1.5 h, allowed to cool, and the product precipitated by the addition of H2O (5 mL). The mixture was filtered, washed with water, and dried, yielding 16 (1.33 mmol) as a brown solid. 1H NMR (400 MHz, d6-DMSO) δ: 8.75 (1H, t, broad), 8.56 (1H, s), 8.21 (1H, s), 7.43 (2H, d, J=8.6 Hz), 7.04 (2H, d, J=8.6), 4.84 (2H, d, J=5.8), 3.88 (3H, s).

후처리

  1. temperatureto cool
  2. customthe product precipitated by the addition of H2O (5 mL)
  3. filtrationThe mixture was filtered
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-ed92b2d4f1f44faf9f9d2206b77c10c7
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07635695B2

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