Potassium Carbonate → HCID 18446524, 화합물

HRID 1868295노트

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HRID 1868295 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+].Cl[C:18]1[C:23]2[CH:24]=[C:25]([I:27])[S:26][C:22]=2[C:21]([C:28]#[N:29])=[CH:20][N:19]=1>CN1C(=O)CCC1>[I:27][C:25]1[S:26][C:22]2[C:21]([C:28]#[N:29])=[CH:20][N:19]=[C:18]([NH:8][CH2:7][C:6]3[CH:9]=[CH:10][C:3]([O:2][CH3:1])=[CH:4][CH:5]=3)[C:23]=2[CH:24]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 754524-MethoxybenzylamineHCID 18446569HCID 18446569, 화합물

생성물 1

HCID 18446524HCID 18446524, 화합물수율 78.6%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

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온도
80 °C

실험 절차

To NMP (41.3 mL) and 4-methoxybenzylamine (3.66 mL, 28.1 mmol) was added K2CO3 (7.76 g, 56.2 mmol) and 4-chloro-2-iodo-thieno[3,2-c]pyridine-7-carbonitrile 26 (7.52 g, 23.4 mmol). The reaction was heated to 80° C. After 1.5 h, NMP was distilled away under reduced pressure. The resulting solids were suspended in H2O (500 mL) and filtered. The product was recrystallized from 350 mL of toluene to obtain 7.75 g of 27. 1H NMR (400 MHz, d6-DMSO) δ 8.58 (t, J=6 Hz, 1H), 8.35 (s, 1H), 8.17 (s, 1H), 7.28 (d, J=9 Hz, 2H), 6.89 (d, J=9 Hz, 2H), 4.68 (d, J=6 Hz, 2H), 3.37 (s, 3H).

후처리

  1. distillationNMP was distilled away under reduced pressure
  2. filtrationfiltered
  3. customThe product was recrystallized from 350 mL of toluene

출처 및 근거

ORD 기록
ord-ed55b1d240df441bb9def98b47dcab53
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07635695B2

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