Pyridine → 5-(Chloromethyl)pyridine-2-carbonitrile
반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9]O)=[CH:5][N:4]=1)#[N:2].N1C=CC=CC=1.C1(C)C=CC(S([Cl:26])(=O)=O)=CC=1>C1(C)C=CC=CC=1>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][Cl:26])=[CH:5][N:4]=1)#[N:2]참가 물질
5
실험 절차
2-Cyano-5-hydroxymethylpyridine (13.4 g) and pyridine (8.7 g) were dissolved in toluene (150 ml), and a solution of p-toluenesufonyl chloride (19.1 g) in toluene (50 ml) was added dropwise at room temperature to the solution. After the addition, the mixture was gradually heated, and stirred at 70° to 80° C. for 4 hours. The reaction mixture was cooled to room temperature, and washed with water. The organic layer was dried. Toluene was distilled off under reduced pressure. The residue was purified by silica gel column chromatography to give 2-cyano-5-pyridylmethyl chloride (7.7 g) as colorless crystals.
후처리
- additionAfter the addition
- temperaturethe mixture was gradually heated
- washwashed with water
- customThe organic layer was dried
- distillationToluene was distilled off under reduced pressure
- customThe residue was purified by silica gel column chromatography
출처 및 근거
- ORD 기록
- ord-777a8f7cac9045b4908dbc2663417489
- 출처 데이터셋
- uspto-grants-1988_09
- 특허 번호
- US04772620
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