Water → 1'-[6-(1H-imidazol-1-yl)pyridazin-3-yl]spiro[1-benzofuran-3,4'-piperidine]

HRID 2036120ノート

反応式

HRID 2036120 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([N:8]2[CH:12]=[CH:11][N:10]=[CH:9]2)=[CH:6][CH:7]=1.[NH:13]1[CH2:18][CH2:17][C:16]2([C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[O:20][CH2:19]2)[CH2:15][CH2:14]1.C(N(CC)CC)C.O>CN(C)C=O>[N:8]1([C:5]2[N:4]=[N:3][C:2]([N:13]3[CH2:18][CH2:17][C:16]4([C:22]5[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=5[O:20][CH2:19]4)[CH2:15][CH2:14]3)=[CH:7][CH:6]=2)[CH:12]=[CH:11][N:10]=[CH:9]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 27709033-Chloro-6-(1H-imidazol-1-yl)pyridazineHCID 151870462H-Spiro(1-benzofuran-3,4'-piperidine)

生成物 1

HCID 866399991'-[6-(1H-imidazol-1-yl)pyridazin-3-yl]spiro[1-benzofuran-3,4'-piperidine]収率 74%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
160 °C

実験手順

3-Chloro-6-(1H-imidazol-1-yl)pyridazine (180 mg), spiro[1-benzofuran-3,4′-piperidine] (200 mg) and triethylamine (0.42 mL) were dissolved in N,N-dimethylformamide (1 mL), and the solution was stirred at 160° C. under irradiation of microwave for 20 min. Water (10 mL) was added, and the resulting precipitate was collected by filtration, and recrystallized from ethyl acetate-hexane to give the object product (245 mg, 74%).

後処理

  1. filtrationthe resulting precipitate was collected by filtration
  2. customrecrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-6c112ab5e275487dbb23016523003941
出典データセット
uspto-grants-2013_11
特許番号
US08575167B2

反応ノート

読み込み中…