Triethylamine → HCID 178506202、化合物

HRID 42229

反応式

HRID 42229 の反応式
Cl[C:2]1[N:7]=[N:6][C:5]([Cl:8])=[C:4]2[NH:9][CH:10]=[N:11][C:3]=12.C(N(CC)CC)C.[F:19][C:20]([F:34])([F:33])[C:21]1[CH:22]=[CH:23][C:24]([N:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)=[N:25][CH:26]=1>O1CCOCC1>[Cl:8][C:5]1[N:6]=[N:7][C:2]([N:30]2[CH2:31][CH2:32][N:27]([C:24]3[CH:23]=[CH:22][C:21]([C:20]([F:34])([F:19])[F:33])=[CH:26][N:25]=3)[CH2:28][CH2:29]2)=[C:3]2[N:11]=[CH:10][NH:9][C:4]=12

参加物

5

反応物 3

HCID 8471TriethylamineHCID 6676181-(5-Trifluoromethyl-pyridin-2-yl)-piperazineHCID 53028254,7-Dichloro-1H-imidazo(4,5-d)pyridazine

生成物 1

HCID 178506202HCID 178506202、化合物収率 57%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

4,7-Dichloro-1H-imidazo[4,5-d]pyridazine (250 mg, 1.32 mmol) is combined with triethylamine (270 μL), dioxane (2 mL), and 1-(5-Trifluoromethyl-pyridin-2-yl)-piperazine (290 mg, 1.26 mmol). The reaction mixture is heated to 80° C. for 70 h. Concentrate in vacuo to remove dioxane. The residue is purified by flash chromatography on silica gel (MeOH/CH2Cl2) to afford the title compound (176 mg, 57%).

後処理

  1. concentrationConcentrate in vacuo
  2. customto remove dioxane
  3. customThe residue is purified by flash chromatography on silica gel (MeOH/CH2Cl2)

出典と根拠

ORDレコード
ord-8193877e583f4d049808c1e95cd14127
出典データセット
uspto-grants-2013_09
特許番号
US08536168B2

関連ノート

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