ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → p-Nitrobenzyl 7-[2-(5-amino-1,2,4-thiadiazol-3-yl)-2-ethoxyiminoacetamido]-3-vinylthio-3-cephem-4-carboxylate

HRID 704279
ノート
印刷プレビュー

反応式

HRID 704279 の反応式
C(N[CH:5]([CH3:7])C)(C)C.C([Li])CCC.C(OC1[S:20]CCO1)C.[NH2:21][C:22]1[S:26][N:25]=[C:24]([C:27](=[N:58][O:59][CH2:60][CH3:61])[C:28]([NH:30][CH:31]2[C:56](=[O:57])[N:33]3[C:34]([C:43]([O:45][CH2:46][C:47]4[CH:52]=[CH:51][C:50]([N+:53]([O-:55])=[O:54])=[CH:49][CH:48]=4)=O)=[C:35](OS(C)(=O)=O)[CH2:36][S:37][C@H:32]23)=[O:29])[N:23]=1.Cl>O1CCCC1.CCCCCC>[NH2:21][C:22]1[S:26][N:25]=[C:24]([C:27](=[N:58][O:59][CH2:60][CH3:61])[C:28]([NH:30][CH:31]2[C:56](=[O:57])[N:33]3[C:34]([C:43]([O:45][CH2:46][C:47]4[CH:48]=[CH:49][C:50]([N+:53]([O-:55])=[O:54])=[CH:51][CH:52]=4)=[S:20])=[C:35]([CH:5]=[CH2:7])[CH2:36][S:37][C@H:32]23)=[O:29])[N:23]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 7912DiisopropylamineHCID 51360032-Ethoxy-1,3-oxathiolaneHCID 131716148p-Nitrobenzyl 7-[2-(5-amino-1,2,4-thiadiazol-3-yl)-2-ethoxyiminoacetamido]-3-mesyloxy-3-cephem-4-carboxylateHCID 178418339Butyllithium

生成物 1

HCID 131716166
p-Nitrobenzyl 7-[2-(5-amino-1,2,4-thiadiazol-3-yl)-2-ethoxyiminoacetamido]-3-vinylthio-3-cephem-4-carboxylate

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒3 回HCID 8058Hexane溶媒

反応条件

温度
0 °C

実験手順

To a solution of N,N-diisopropylamine (0.65 ml) in tetrahydrofuran (7 ml) was added 1.55M n-butyllithium in n-hexane (2.88 ml) at -20°~-15° C. The mixture was stirred for 30 minutes at 0° C. To the solution was added a solution of 2-ethoxy-1,3-oxathiolane (642 mg) in tetrahydrofuran (2 ml) at -60° C., and the resultant mixture was stirred for 30 minutes at the same temperature. The solution was added to a solution of p-nitrobenzyl 7-[2-(5-amino-1,2,4-thiadiazol-3-yl)-2-ethoxyiminoacetamido]-3-mesyloxy-3-cephem-4-carboxylate (syn isomer) (2 g) in tetrahydrofuran (30 ml) at -62° C. After the mixture was stirred for 15 minutes at the same temperature, 1N hydrochloric acid (5 ml) was added thereto. The mixture was allowed to warm up till 0° C. and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was subjected to column chromatography on silica gel and eluted with a mixture of ethyl acetate and chloroform (1:2). The fractions containing the object compound were combined and concentrated in vacuo to give p-nitrobenzyl 7-[2-(5-amino-1,2,4-thiadiazol-3-yl)-2-ethoxyiminoacetamido]-3-vinylthio-3-cephem-4-carboxylate (syn isomer) (805 mg).

後処理

  1. additionwas added
  2. temperatureto warm up till 0° C.
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. washeluted with a mixture of ethyl acetate and chloroform (1:2)
  8. additionThe fractions containing the object compound
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4ef68b9063724738bdbc942ed64b4785
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04985555

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート