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Water → (2R,4R)-1-allyloxycarbonyl-4-methanesulfonyloxy-2-{2(5-methoxymethylimidazol-1-yl)ethyl}pyrrolidine

HRID 975704
ノート
印刷プレビュー

反応式

HRID 975704 の反応式
[CH2:1]([O:4][C:5]([N:7]1[CH2:11][C@H:10]([OH:12])[CH2:9][C@H:8]1[CH2:13][CH2:14][N:15]1[C:19]([CH2:20][O:21][CH3:22])=[CH:18][N:17]=[CH:16]1)=[O:6])[CH:2]=[CH2:3].C(N(CC)CC)C.[CH3:30][S:31](Cl)(=[O:33])=[O:32].O>C(OCC)(=O)C>[CH2:1]([O:4][C:5]([N:7]1[CH2:11][C@H:10]([O:12][S:31]([CH3:30])(=[O:33])=[O:32])[CH2:9][C@H:8]1[CH2:13][CH2:14][N:15]1[C:19]([CH2:20][O:21][CH3:22])=[CH:18][N:17]=[CH:16]1)=[O:6])[CH:2]=[CH2:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 53905519(2R,4R)-1-allyloxycarbonyl-4-hydroxy-2-{2-(5-methoxymethylimidazol-1-yl)ethyl}pyrrolidine

生成物 1

HCID 22870378(2R,4R)-1-allyloxycarbonyl-4-methanesulfonyloxy-2-{2(5-methoxymethylimidazol-1-yl)ethyl}pyrrolidine

試薬・触媒・溶媒 1

HCID 8857
Ethyl Acetate
溶媒

実験手順

To a solution of (2R,4R)-1-allyloxycarbonyl-4-hydroxy-2-{2-(5-methoxymethylimidazol-1-yl)ethyl}pyrrolidine (3.63 g) in ethyl acetate (40 ml) were added successively triethylamine (2.29 ml) and methanesulfonyl chloride (1.09 ml) with stirring under ice-cooling. The mixture was stirred at the same temperature for 1 hour. To the reaction mixture was added water (20 ml). The organic layer was separated and washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and evaporated in vacuo to give a residue. The residue was chromatographed on silica gel (150 g) eluting with a mixture of chloroform and methanol (19:1, V/V). The fractions containing the desired compound were collected and evaporated in vacuo to give (2R,4R)-1-allyloxycarbonyl-4-methanesulfonyloxy-2-{2(5-methoxymethylimidazol-1-yl)ethyl}pyrrolidine (3.85 g).

後処理

  1. temperaturecooling
  2. stirringThe mixture was stirred at the same temperature for 1 hour
  3. customThe organic layer was separated
  4. washwashed with saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated in vacuo
  7. customto give a residue
  8. customThe residue was chromatographed on silica gel (150 g)
  9. washeluting with a mixture of chloroform and methanol (19:1, V/V)
  10. additionThe fractions containing the desired compound
  11. customwere collected
  12. customevaporated in vacuo

出典と根拠

ORDレコード
ord-0fb31f0d8f624e49a719f0733fe408e1
出典データセット
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05608056

反応ノート

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