Pyridine → HCID 20263705、化合物
反応式
[F:1][C:2]([F:9])([F:8])[C:3]1[NH:7][N:6]=[N:5][N:4]=1.[C:10](Cl)(=[O:26])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].N1C=CC=CC=1>C(#N)C>[C:10]([N:4]1[C:3]([C:2]([F:9])([F:8])[F:1])=[N:7][N:6]=[N:5]1)(=[O:26])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]参加物
5
反応条件
- 温度
- 5 °C
実験手順
6.9 g of 5-trifluoromethyl-1,2,3,4-tetrazole and 13.7 g of palmitoyl chloride were dissolved in 100 ml of acetonitrile while cooling with ice and to the solution was added dropwise 4.5 ml of pyridine over a period of about 10 minutes. After the completion of the dropwise addition, the mixture was stirred at about 5° C. for 30 minutes and then at room temperature for 1 hour, and to the mixture was added dropwise about 100 ml of ice water. The crystals thus-deposited were collected by filtration to obtain 8.2 g of 1-hexadecanoyl-5-trifluoromethyl-1,2,3,4 -tetrazole. A melting point was 66° to 69° C.
後処理
- temperaturewhile cooling with ice and to the solution
- additionAfter the completion of the dropwise addition
- waitat room temperature for 1 hour
- filtrationThe crystals thus-deposited were collected by filtration
出典と根拠
- ORDレコード
- ord-8c5e73afbf9a4faea9e53a36551afd1a
- 出典データセット
- uspto-grants-1985_10
- 特許番号
- US04546075
反応ノート
読み込み中…