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Acetic Acid → HCID 15056146、化合物

HRID 1590489
ノート
印刷プレビュー

反応式

HRID 1590489 の反応式
C([S:4][C@@H:5]1[CH2:9][N:8]([C:10]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=2)=[O:11])[C@H:7]([CH2:23][N:24]2[CH2:28][CH2:27][N:26]([CH3:29])[C:25]2=[O:30])[CH2:6]1)(=O)C.C[O-].[Na+].C(O)(=O)C>CO.C(OCC)(=O)C.O1CCCC1>[SH:4][C@@H:5]1[CH2:9][N:8]([C:10]([O:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=2)=[O:11])[C@H:7]([CH2:23][N:24]2[CH2:28][CH2:27][N:26]([CH3:29])[C:25]2=[O:30])[CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 176Acetic AcidHCID 10942334Sodium MethoxideHCID 15056145(2S,4S)-4-acetylthio-2-(3-methyl-2-oxoimidazolidin-1-yl)methyl-1-(4-nitrobenzyloxycarbonyl)-pyrrolidine

生成物 1

HCID 15056146HCID 15056146、化合物収率 79.1%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒2 回
HCID 8028
Tetrahydrofuran
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of (2S,4S)-4-acetylthio-2-(3-methyl-2-oxoimidazolidin-1-yl)methyl-1-(4-nitrobenzyloxycarbonyl)-pyrrolidine (1.72 g) in methanol (40 ml) was added 28% sodium methoxide in methanol solution (0.83 ml) and the mixture was stirred under ice-cooling for 30 minutes. Acetic acid (0.25 ml) was added to the reaction mixture at the same temperature. The mixture was evaporated in vacuo to give a residue. The residue was dissolved in a mixture of ethyl acetate (80 ml) and tetrahydrofuran (30 ml) and the solution was washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and evaporated in vacuo. The resulting residue was chromatographed on silica gel (100 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 (2S,4S)-4-mercapto-2-(3-methyl-2-oxoimidazolidin-1-yl)methyl-1-(4-nitrobenzyloxycarbonyl)pyrrolidine (1.23 g).

後処理

  1. temperaturecooling for 30 minutes
  2. customThe mixture was evaporated in vacuo
  3. customto give a residue
  4. washthe solution was washed with saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated in vacuo
  7. customThe resulting residue was chromatographed on silica gel (100 g)
  8. washeluting with a mixture of chloroform and methanol (19:1, V/V)
  9. additionThe fractions containing the desired compound
  10. customwere collected
  11. customevaporated in vacuo

出典と根拠

ORDレコード
ord-3aa849999bc24b3cb159744eff6d85b4
出典データセット
uspto-grants-1993_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05202437

反応ノート

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