6-chloro-2-methyl-9-(beta-D-ribofuranosyl)-9H-purine → HCID 178433181、化合物

HRID 1086803ノート

反応式

HRID 1086803 の反応式
Cl[C:2]1[N:10]=[C:9]([CH3:11])[N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[C@@H:12]1[O:18][C@H:17]([CH2:19][OH:20])[C@@H:15]([OH:16])[C@H:13]1[OH:14].Cl.[NH2:22][C@H:23]1[CH2:28][CH2:27][C@H:26]([OH:29])[CH2:25][CH2:24]1>C(O)(C)C>[OH:29][C@H:26]1[CH2:27][CH2:28][C@H:23]([NH:22][C:2]2[C:3]3[N:4]=[CH:5][N:6]([C:7]=3[N:8]=[C:9]([CH3:11])[N:10]=2)[C@@H:12]2[O:18][C@H:17]([CH2:19][OH:20])[C@@H:15]([OH:16])[C@H:13]2[OH:14])[CH2:24][CH2:25]1

参加物

4

反応物 2

HCID 542785016-chloro-2-methyl-9-(beta-D-ribofuranosyl)-9H-purineHCID 178479278HCID 178479278、化合物

生成物 1

HCID 178433181HCID 178433181、化合物収率 79.1%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 6-chloro-2-methyl-9-(β-D-ribofuranosyl)-9H-purine (902 mg), trans-4-aminocyclohexanol hydrochloride (1.14 g) and DEA (1.94 g) in isopropanol (50 ml) was heated at reflux with stirring under nitrogen for 17 h. The resulting cooled reaction mixture was adsorbed onto silica (Merck 9385) and purified by column chromatography on silica (Merck 9385) eluting with System B (10:1 then 8:1) to give the title compound (0.9 g) as a solid.

後処理

  1. temperaturewas heated
  2. temperatureat reflux
  3. temperatureThe resulting cooled
  4. customreaction mixture
  5. custompurified by column chromatography on silica (Merck 9385)
  6. washeluting with System B (10:1

出典と根拠

ORDレコード
ord-eee0310c533c4584987382826d592722
出典データセット
uspto-grants-1991_07
特許番号
US05032583

反応ノート

読み込み中…