Triethylamine → HCID 68995395、化合物

HRID 660500

反応式

HRID 660500 の反応式
[CH:1]([N:3]1[CH:7]=[N:6][CH:5]=[N:4]1)=[CH2:2].[CH2:8]([O:15][C:16]1[CH:21]=[C:20](I)[CH:19]=[CH:18][C:17]=1[N:23]1[S:27](=[O:29])(=[O:28])[NH:26][C:25](=[O:30])[CH2:24]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(N(CC)CC)C>C(#N)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:8]([O:15][C:16]1[CH:21]=[C:20](/[CH:2]=[CH:1]/[N:3]2[CH:7]=[N:6][CH:5]=[N:4]2)[CH:19]=[CH:18][C:17]=1[N:23]1[S:27](=[O:29])(=[O:28])[NH:26][C:25](=[O:30])[CH2:24]1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 5652611-Vinyl-1,2,4-triazoleHCID 688386435-(2-Benzyloxy-4-iodophenyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one

生成物 1

HCID 68995395HCID 68995395、化合物

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 6342Acetonitrile溶媒

反応条件

温度
110 °C

実験手順

A mixture of 1-vinyl-1,2,4-triazole (0.100 g, 1.06 mmol), 5-(2-benzyloxy-4-iodophenyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one (0.236 g, 0.531 mmol), palladium acetate (0.024 g, 0.107 mmol), triethylamine (0.295 mL, 2.09 mmol) in acetonitrile is heated in a microwave apparatus at 110° C. for 30 min. The mixture is filtered over Celite, washed with acetonitrile, and concentrated. The residue is purified by column chromatography using a gradient of 10-60% EtOH/water as eluent to afford the title compound: (M−1)−=410.

後処理

  1. filtrationThe mixture is filtered over Celite
  2. washwashed with acetonitrile
  3. concentrationconcentrated
  4. customThe residue is purified by column chromatography

出典と根拠

ORDレコード
ord-cabf7022cee74f69b02eee0ecfeaffcf
出典データセット
uspto-grants-2011_12
特許番号
US08084448B2

関連ノート

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