1H-Benzimidazole, 1-methyl- → N-Methyl-N'-2-pyridylbenzimidazolium iodide

HRID 39316

반응식

HRID 39316 반응식
[I:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[CH3:8][N:9]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[N:11]=[CH:10]1>CC(C)=O>[I-:1].[CH3:8][N+:9]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[N:11]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=2)[CH:10]=1

참가 물질

4

반응물 2

HCID 958901H-Benzimidazole, 1-methyl-HCID 2211262-Iodopyridine

생성물 1

HCID 12434486N-Methyl-N'-2-pyridylbenzimidazolium iodide

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 2-iodopyridine (2.0 g, 9.8 mmol) and 1-methylbenzimidazole (1.29 g, 9.8 mmol) was kept neat at 140° C. for 72 h. After cooling to ca 50° C., acetone was added and the resulting solid was filtered and washed with acetone and ether. Yield: 826 mg (25%). 1H NMR (DMSO-d6): δ 10.48 (s, 1H, NCHN), 8.79 (d, 1H), 8.47-8.49 (m, 1H), 8.27-8.32 (dt, 1H), 8.14-8.16 (m, 1H), 8.04 (d, 1H), 7.77-7.82 (m, 2H), 7.71-7.74 (dd, 1H), 4.20 (s, 3H, CH3). This ligand was pure by 1H-NMR and was used without further purification.

후처리

  1. temperatureAfter cooling to ca 50° C.
  2. filtrationthe resulting solid was filtered
  3. washwashed with acetone and ether
  4. customwas used without further purification

출처 및 근거

ORD 기록
ord-e7e502ae3d5e48b4bfd22d460649daae
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524903B2

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