Triethylamine → 2-(Chloromethyl)-1-(2,6-dichlorobenzyl)-4-nitro-1H-imidazole

HRID 714633ノート

反応式

HRID 714633 の反応式
[Cl:1][C:2]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:3]=1[CH2:4][N:5]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[N:7]=[C:6]1[CH2:13]O.C(N(CC)CC)C.S(Cl)([Cl:29])=O>ClCCl>[Cl:29][CH2:13][C:6]1[N:5]([CH2:4][C:3]2[C:2]([Cl:1])=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:19])[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[N:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24386Thionyl Chloride2 回HCID 67410386[1-(2,6-Dichlorobenzyl)-4-nitro-1H-imidazol-2-yl]methanol

生成物 1

HCID 674099292-(Chloromethyl)-1-(2,6-dichlorobenzyl)-4-nitro-1H-imidazole

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

210 mg (0.70 mmol) of the compound from Example 37A were dissolved in 10 ml of dichloromethane, and 145 μl (1.04 mmol) of triethylamine and 61 μl (0.83 mmol) of thionyl chloride were added at 0° C. The mixture was stirred at RT for 24 h. A further 200 μl (2.72 mmol) of thionyl chloride were then added, and the mixture was stirred under reflux for 15 min. Under reduced pressure, the reaction mixture was then freed from all volatile components. This gave, in a purity of 88%, 200 mg (80% of theory) of the target compound, which was reacted further without any further purification.

後処理

  1. stirringthe mixture was stirred
  2. temperatureunder reflux for 15 min
  3. customThis gave, in a purity of 88%, 200 mg (80% of theory) of the target compound, which was reacted further without any further purification

出典と根拠

ORDレコード
ord-7ca9cbf52d864006b20986c798521ac7
出典データセット
uspto-grants-2015_11
特許番号
US09187466B2

反応ノート

読み込み中…