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

Dichloromethane → (3R,5R,6R)-3-(3-amino-2-oxoimidazolidin-1-yl)-3-(p-nitrobenzyloxycarbonyl)-7-oxo-6-phenylacetamido-4-thia-1-azabicyclo[3.2.0] heptane

HRID 1463439
ノート
印刷プレビュー

反応式

HRID 1463439 の反応式
C(Cl)Cl.C(=[N:11][N:12]1[CH2:16][CH2:15][N:14]([C@@:17]2([C:35]([O:37][CH2:38][C:39]3[CH:44]=[CH:43][C:42]([N+:45]([O-:47])=[O:46])=[CH:41][CH:40]=3)=[O:36])[S:23][C@H:22]3[N:19]([C:20](=[O:34])[C@H:21]3[NH:24][C:25](=[O:33])[CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[CH2:18]2)[C:13]1=[O:48])C1C=CC=CC=1.[N+](C1C=C([N+]([O-])=O)C=CC=1NN)([O-])=O.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[NH2:11][N:12]1[CH2:16][CH2:15][N:14]([C@@:17]2([C:35]([O:37][CH2:38][C:39]3[CH:40]=[CH:41][C:42]([N+:45]([O-:47])=[O:46])=[CH:43][CH:44]=3)=[O:36])[S:23][C@H:22]3[N:19]([C:20](=[O:34])[C@H:21]3[NH:24][C:25](=[O:33])[CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[CH2:18]2)[C:13]1=[O:48]
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 6344DichloromethaneHCID 521998p-Toluenesulfonic acid monohydrateHCID 3772977(2,4-Dinitrophenyl)hydrazineHCID 54119937(3R,5R,6R)-3-(3-benzylideneamino-2-oxoimidazolidin-1-yl)-3-(p-nitrobenzyloxycarbonyl)-7-oxo-6-phenylacetamido-4-thia-1-azabicyclo[3.2.0]heptane

生成物 1

HCID 18649726
(3R,5R,6R)-3-(3-amino-2-oxoimidazolidin-1-yl)-3-(p-nitrobenzyloxycarbonyl)-7-oxo-6-phenylacetamido-4-thia-1-azabicyclo[3.2.0] heptane
収率 60.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In a mixed solvent consisting of 30 ml of methylene chloride and 15 ml of methanol was dissolved 3.00 g of (3R,5R,6R)-3-(3-benzylideneamino-2-oxoimidazolidin-1-yl)-3-(p-nitrobenzyloxycarbonyl)-7-oxo-6-phenylacetamido-4-thia-1-azabicyclo[3.2.0]heptane. To the solution were added 1.89 g of 2,4-dinitrophenylhydrazine and 850 mg of p-toluenesulfonic acid monohydrate in this order. The mixture was stirred at room temperature for 1.5 hours. Then, the insolubles were removed by filtration. The filtrate was concentrated under reduced pressure. The residue was mixed with a mixed solvent consisting of 30 ml of methylene chloride and 7 ml of methanol. The insolubles were removed by filtration. The filtrate was concentrate under reduced pressure. The residue was purified by column chromatography (eluant: chloroform/methanol=100/1 to 25/1) to obtain 1.56 g (yield: 60.5%) of (3R,5R,6R)-3-(3-amino-2-oxoimidazolidin-1-yl)-3-(p-nitrobenzyloxycarbonyl)-7-oxo-6-phenylacetamido-4-thia-1-azabicyclo[3.2.0] heptane.

後処理

  1. customThen, the insolubles were removed by filtration
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. additionThe residue was mixed with a mixed solvent
  4. customThe insolubles were removed by filtration
  5. concentrationThe filtrate was concentrate under reduced pressure
  6. customThe residue was purified by column chromatography (eluant: chloroform/methanol=100/1 to 25/1)

出典と根拠

ORDレコード
ord-a3334a83d5884897901d1a637e653b53
出典データセット
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05300497

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート