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

Phosphoric Acid → HCID 70582695、化合物

HRID 261711
ノート
印刷プレビュー

反応式

HRID 261711 の反応式
[C:1]([O:5][C:6]([NH:8][C@@H:9]1[C:21](=[O:22])[N:11]2[C:12]([C:18]([O-:20])=[O:19])=[C:13]([CH2:16][OH:17])[CH2:14][S:15][C@H:10]12)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Na+].[C:24]([N:29]1[C:39](=[O:40])[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[S:30]1(=[O:32])=[O:31])([O:26][CH2:27][CH3:28])=[O:25].C(N(CC)CC)C.P(=O)(O)(O)O>CN(C)C=O.O.C(OCC)(=O)C.C1(C)C=CC=CC=1>[C:1]([O:5][C:6]([NH:8][C@@H:9]1[C:21](=[O:22])[N:11]2[C:12]([C:18]([OH:20])=[O:19])=[C:13]([CH2:16][O:17][C:39](=[O:40])[C:38]3[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=3[S:30](=[O:32])(=[O:31])[NH:29][C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:14][S:15][C@H:10]12)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 1004Phosphoric AcidHCID 8471Triethylamine2 回HCID 227704Ethyl 3-oxo-1,2-benzothiazole-2(3h)-carboxylate 1,1-dioxideHCID 70582610Sodium 7beta-(t-butoxycarbonyl)amino-3-hydroxymethyl-3-cephem-4-carboxylate

生成物 1

HCID 70582695HCID 70582695、化合物収率 47%

試薬・触媒・溶媒 4

HCID 962
Water
溶媒
HCID 1140Toluene溶媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

In dimethylformamide (20 ml) is dissolved sodium 7β-(t-butoxycarbonyl)amino-3-hydroxymethyl-3-cephem-4-carboxylate (3.20 g), followed by the addition of N-carboethoxysaccharin (3.20 g) and triethylamine (2.0 ml). The solution is stirred for one hour at room temperature and, after the addition of triethylamine (2.0 ml), stirred further for one hour. The solution is poured into toluene (1 L) and the resultant precipitate is collected by filtration, washed with toluene and dried. The powder thus obtained is dissolved in water (30 ml). After the addition of ethyl acetate (200 ml), the solution is adjusted to pH 4.0 with diluted phosphoric acid. After separation, the ethyl acetate solution is washed with water, dried over anhydrous sodium sulfate and concentrated. To the concentrate (30 ml), ether (200 ml) is added under stirring and the resultant precipitate is filtered off. The filtrate is concentrated under reduced pressure and to the concentrate (30 ml) is added carbon tetrachloride (100 ml). The resultant precipitate is collected by filtration, washed with carbon tetrachloride and dried over phosphorus pentoxide. The procedure provides 7β-(t-butoxycarbonyl)amino-3-[2-(N-carboethoxysulfamoyl)benzoyloxy]methyl-3-cephem-4-carboxylic acid (2.50 g).

後処理

  1. stirringstirred further for one hour
  2. filtrationthe resultant precipitate is collected by filtration
  3. washwashed with toluene
  4. customdried
  5. customThe powder thus obtained
  6. customAfter separation
  7. washthe ethyl acetate solution is washed with water
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated
  10. concentrationTo the concentrate (30 ml), ether (200 ml)
  11. additionis added
  12. stirringunder stirring
  13. filtrationthe resultant precipitate is filtered off
  14. concentrationThe filtrate is concentrated under reduced pressure
  15. concentrationto the concentrate (30 ml)
  16. additionis added carbon tetrachloride (100 ml)
  17. filtrationThe resultant precipitate is collected by filtration
  18. washwashed with carbon tetrachloride
  19. dry with materialdried over phosphorus pentoxide

出典と根拠

ORDレコード
ord-81ea8bef42224603a4b8b5c508e468d7
出典データセット
uspto-grants-1979_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04166178

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