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Cesium carbonate → 4-Allyl-5-(4-chlorophenyl)-2-{[1-(2,6-dichlorobenzyl)-4-nitro-1H-imidazol-2-yl]methyl}-2,4-dihydro-3H-1,2,4-triazol-3-one

HRID 714720
ノート
印刷プレビュー

反応式

HRID 714720 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]([CH2:14][CH:15]=[CH2:16])[C:10](=[O:13])[NH:11][N:12]=2)=[CH:4][CH:3]=1.Cl[CH2:18][C:19]1[N:20]([CH2:27][C:28]2[C:33]([Cl:34])=[CH:32][CH:31]=[CH:30][C:29]=2[Cl:35])[CH:21]=[C:22]([N+:24]([O-:26])=[O:25])[N:23]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C>[CH2:14]([N:9]1[C:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)=[N:12][N:11]([CH2:18][C:19]2[N:20]([CH2:27][C:28]3[C:29]([Cl:35])=[CH:30][CH:31]=[CH:32][C:33]=3[Cl:34])[CH:21]=[C:22]([N+:24]([O-:26])=[O:25])[N:23]=2)[C:10]1=[O:13])[CH:15]=[CH2:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 497656025-(4-chlorophenyl)-4-allyl-2,4-dihydro-3H-1,2,4-triazol-3-oneHCID 674099292-(Chloromethyl)-1-(2,6-dichlorobenzyl)-4-nitro-1H-imidazole

生成物 1

HCID 699405054-Allyl-5-(4-chlorophenyl)-2-{[1-(2,6-dichlorobenzyl)-4-nitro-1H-imidazol-2-yl]methyl}-2,4-dihydro-3H-1,2,4-triazol-3-one

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
80 °C

実験手順

110 mg (0.47 mmol) of the compound from Example 12A were dissolved in 10 ml of DMF, and 150 mg (0.47 mmol) of the compound from Example 41A and 229 mg (0.70 mmol) of cesium carbonate were added. The mixture was stirred at 80° C. for 16 h. After cooling to RT, the reaction mixture was added to about 25 ml of ice-water and stirred for 10 min. This resulted in the formation of a precipitate which was filtered off with suction and washed with water. The solid was dried under high vacuum. This gave 120 mg (44% of theory) of the target compound of a purity of 90%.

後処理

  1. temperatureAfter cooling to RT
  2. stirringstirred for 10 min
  3. customThis resulted in the formation of a precipitate which
  4. filtrationwas filtered off with suction
  5. washwashed with water
  6. customThe solid was dried under high vacuum

出典と根拠

ORDレコード
ord-c83edcda6f7a4a998fd4583f8eb83acd
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09187466B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート