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

Methanol → Benzhydryl 7-Amino-3-chloromethyl-3-cephem-4-carboxylate

HRID 1681450
ノート
印刷プレビュー

反応式

HRID 1681450 の反応式
N1C=CC=CC=1.C1(CC([NH:16][CH:17]2[C:42](=[O:43])[N:19]3[C:20]([C:26]([O:28][CH:29]([C:36]4[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=4)[C:30]4[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=4)=[O:27])=[C:21]([CH2:24]O)[CH2:22][S:23][C@H:18]23)=O)C=CC=CC=1.P(Cl)(Cl)(Cl)(Cl)[Cl:45].CO>C(Cl)Cl>[NH2:16][CH:17]1[C:42](=[O:43])[N:19]2[C:20]([C:26]([O:28][CH:29]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)=[O:27])=[C:21]([CH2:24][Cl:45])[CH2:22][S:23][C@H:18]12
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

6

反応物 4

HCID 887MethanolHCID 1049PyridineHCID 24819Phosphorus pentachlorideHCID 13339796Benzhydryl 3-hydroxymethyl-7-phenylacetamido-3-cephem-4-carboxylate

生成物 1

HCID 13239626Benzhydryl 7-Amino-3-chloromethyl-3-cephem-4-carboxylate

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

反応条件

温度
-20 °C

実験手順

19.64 ml (0.242 mol) of pyridine are added to a suspension of 50 g (0.0972 mol) of benzhydryl 7-phenylacetamido-3-hydroxymethyl-3-cephem-4-carboxylate in 500 ml of methylene chloride at room temperature. After cooling to -20° C., 40.48 g (0.0972 mol) of phosphorus pentachloride are added and the mixture is stirred at -20° C. for 5 minutes. The mixture is warmed to 0° C. with an icebath and stirred for 10 minutes, and is then warmed to 15° C. with a waterbath and stirred for 1 hour. Thereafter, the mixture is cooled to -70° C. and 720 ml of cold methanol are quickly added The mixture is then stirred at -70° C. for 5 minutes, at 0° C. for 10 minutes and at +15° C. for 25 minutes. The solution is subsequently concentrated to a high degree in vacuo and 1,400 ml of saturated sodium bicarbonate solution are added. The solution is extracted three times with methylene chloride and the organic phase is dried with sodium sulphate and concentrated in vacuo. The crude product is chromatographed on 500 g of silica gel 60 (0.04-0.063 mm) with methylene chloride.

後処理

  1. temperatureThe mixture is warmed to 0° C. with an icebath
  2. stirringstirred for 10 minutes
  3. temperatureis then warmed to 15° C. with a waterbath
  4. stirringstirred for 1 hour
  5. temperatureThereafter, the mixture is cooled to -70° C.
  6. stirringis then stirred at -70° C. for 5 minutes, at 0° C. for 10 minutes and at +15° C. for 25 minutes
  7. concentrationThe solution is subsequently concentrated to a high degree in vacuo and 1,400 ml of saturated sodium bicarbonate solution
  8. additionare added
  9. extractionThe solution is extracted three times with methylene chloride
  10. dry with materialthe organic phase is dried with sodium sulphate
  11. concentrationconcentrated in vacuo
  12. customThe crude product is chromatographed on 500 g of silica gel 60 (0.04-0.063 mm) with methylene chloride

出典と根拠

ORDレコード
ord-f7fa88ce9c704db4b8df998686534428
出典データセット
uspto-grants-1992_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05171854

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