Triethylamine → 2-chloro-5-isocyanatopyridine
反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5](C(O)=O)=[CH:4][N:3]=1.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:18])C=CC=CC=1.C([N:30]([CH2:33]C)CC)C>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([N:30]=[C:33]=[O:18])=[CH:4][N:3]=1参加物
5
実験手順
To a suspension of 6-chloro-nicotinic acid (0.468 g, 3 mmol) (Aldrich) in toluene (15 mL) was added diphenylphosphoryl azide (0.958 g, 3.5 mmol) (Aldrich), followed by the addition of triethylamine (0.35 g, 3.6 mmol) (Aldrich). The mixture was stirred at room temperature for 30 minutes and the mixture became clear. Then the mixture was heated at 80° C. for 2 hours. The mixture was cooling down to room temperature to give crude 2-chloro-5-Isocyanato-pyridine as 0.2 M solution of toluene and used for the next step without further purification.
後処理
- temperatureThen the mixture was heated at 80° C. for 2 hours
- temperatureThe mixture was cooling down to room temperature
出典と根拠
- ORDレコード
- ord-c1789dabdb66425580facd303df5ee44
- 出典データセット
- uspto-grants-2009_08
- 特許番号
- US07576082B2
反応ノート
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