Iodoethane → HCID 57720231、化合物

HRID 1985840ノート

反応式

HRID 1985840 の反応式
[OH:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][NH:7][C:8]2[N:12]([C@@H:13]3[O:19][C@H:18]([CH2:20][OH:21])[C@@H:16]([OH:17])[C@H:14]3[OH:15])[C:11]3[CH:22]=[CH:23][CH:24]=[CH:25][C:10]=3[N:9]=2)=[CH:4][C:3]=1[O:28][CH2:29][CH2:30][CH2:31][CH2:32][OH:33].C(=O)([O-])[O-].[K+].[K+].[CH2:40](I)[CH3:41]>CN(C)C=O>[CH2:40]([O:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][NH:7][C:8]2[N:12]([C@@H:13]3[O:19][C@H:18]([CH2:20][OH:21])[C@@H:16]([OH:17])[C@H:14]3[OH:15])[C:11]3[CH:22]=[CH:23][CH:24]=[CH:25][C:10]=3[N:9]=2)=[CH:4][C:3]=1[O:28][CH2:29][CH2:30][CH2:31][CH2:32][OH:33])[CH3:41]

参加物

5

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 57720213HCID 57720213、化合物

生成物 1

HCID 57720231HCID 57720231、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
55 °C

実験手順

2-[4-Hydroxy-3-(4-hydroxybutoxy)benzylamino]-1-(β-D-ribofuranosyl)-1H-benzimidazole (30 mg) and potassium carbonate (18 mg) was suspended in N,N-dimethylformamide (0.7 mL). To the mixture was added ethyl iodide (20 μL), and the mixture was stirred at 55° C. for 16 hour. The insoluble material was removed by filtration, and the reaction mixture was concentrated under reduced pressure. The obtained residue was purified by preparative reverse phase column chromatography (Shiseido CAPSELL PAC C18UG80, 5 μm, 20×50 mm, flow rate 30 mL/minutes linear gradient, water/methanol=90/10-10/90) to give the title compound (13 mg).

後処理

  1. customThe insoluble material was removed by filtration
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customThe obtained residue was purified by preparative reverse phase column chromatography (Shiseido CAPSELL PAC C18UG80, 5 μm, 20×50 mm, flow rate 30 mL/minutes linear gradient, water/methanol=90/10-10/90)

出典と根拠

ORDレコード
ord-bb2f603eac6b4a4690cccc1c4edab1a6
出典データセット
uspto-grants-2009_06
特許番号
US07547680B2

反応ノート

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