Hydrogen Sulfide → HCID 178478026、化合物
反応式
[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].C([N:12](CC)CC)C.S.[NH2:18][NH2:19].N([O-])=O.[Na+]>CO>[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]1[NH:5][N:12]=[N:19][N:18]=1参加物
7
実験手順
First, 35.6 mmol of 2-chlorobenzonitrile was dissolved in 50 ml of methanol, and 35.6 mmol of triethylarnine and 105 mmol of hydrogen sulfide were added thereto at room temperature, followed by adding 180 mmol of anhydrous hydrazine and keeping at the reflux temperature for 48 hours. The reaction mixture was evaporated under reduced pressure. The residue was dissolved in 50 ml of 5% hydrochloric acid, and 75 mmol of sodium nitrite was added thereto at 0° C. to cause reaction. After completion of the reaction, the reaction mixture was extracted with ethyl acetate to give 5-(2-chlorophenyl)tetrazole. Yield, 54%
後処理
- customat room temperature
- customThe reaction mixture was evaporated under reduced pressure
- dissolutionThe residue was dissolved in 50 ml of 5% hydrochloric acid
- customat 0° C.
- customreaction
- customAfter completion of the reaction
- extractionthe reaction mixture was extracted with ethyl acetate
出典と根拠
- ORDレコード
- ord-27853476a6b94f57a0de9886991d656d
- 出典データセット
- uspto-grants-1999_02
- 特許番号
- US05874593
反応ノート
読み込み中…