HCID 86632922、化合物 → HCID 86632923、化合物

HRID 1628583ノート

反応式

HRID 1628583 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([OH:34])[C:10]1[N:14]([CH2:15][CH2:16][NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[C:13]2[C:25]([N:29]([CH2:32][CH3:33])[CH2:30][CH3:31])=[CH:26][CH:27]=[CH:28][C:12]=2[N:11]=1>O1CCCC1.[O-2].[Mn+4].[O-2]>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]([C:10]1[N:14]([CH2:15][CH2:16][NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[C:13]2[C:25]([N:29]([CH2:32][CH3:33])[CH2:30][CH3:31])=[CH:26][CH:27]=[CH:28][C:12]=2[N:11]=1)=[O:34]

参加物

4

反応物 1

HCID 86632922HCID 86632922、化合物

生成物 1

HCID 86632923HCID 86632923、化合物収率 81.2%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of tert-butyl (2-{2-[(2,4-dichlorophenyl) (hydroxy)methyl]-7-(diethylamino)-1H-benzimidazol-1-yl}ethyl)carbamate (500 mg, 0.985 mmol) and manganese(IV)oxide (856 mg, 9.85 mmol) in tetrahydrofuran (5 mL) was stirred at room temperature for 4 h, filtered and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with a 0-20% ethyl acetate/n-hexane gradient mixture to give a yellow amorphous solid (404 mg, 0.800 mmol, 81%).

後処理

  1. filtrationfiltered
  2. concentrationconcentrated in vacuo
  3. customThe residue was purified by column chromatography on silica gel eluting with a 0-20% ethyl acetate/n-hexane gradient mixture

出典と根拠

ORDレコード
ord-94af4cbbe01244c4bb0dfeb5f0a8de6d
出典データセット
uspto-grants-2014_07
特許番号
US08785460B2

反応ノート

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