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Pyridine → HCID 21453097、化合物

HRID 1284137
ノート
印刷プレビュー

反応式

HRID 1284137 の反応式
N1C=CC=CC=1.[S:7]([NH:11][C:12]([NH2:14])=[O:13])([CH3:10])(=[O:9])=[O:8].[C:15](Cl)([Cl:17])=[O:16]>ClCCl>[S:7]([NH:11][C:12]([NH:14][C:15]([Cl:17])=[O:16])=[O:13])([CH3:10])(=[O:9])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 6371PhosgeneHCID 19365480Methanesulfonamide, N-(aminocarbonyl)-

生成物 1

HCID 21453097HCID 21453097、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

6.1 parts by volume of pyridine were added dropwise, while cooling, to a mixture of 10.5 parts by weight of N-mesylurea, 60 parts by volume of dichloromethane and 15.0 parts by weight of phosgene, while cooling, and after some hours at 0°C the excess of the phosgene was removed, the precipitate present was filtered off and the filtrate was completely concentrated in vacuo. A viscous oil remained, which had an absorption at 1800 cm-1 in the carbonyl region of the IR-spectrum. The substance was used without further purification for the production of the penicillin.

後処理

  1. temperaturewhile cooling
  2. customafter some hours at 0°C the excess of the phosgene was removed
  3. filtrationthe precipitate present was filtered off
  4. concentrationthe filtrate was completely concentrated in vacuo
  5. customan absorption at 1800 cm-1 in the carbonyl region of the IR-spectrum
  6. customThe substance was used without further purification for the production of the penicillin

出典と根拠

ORDレコード
ord-f213e09676c84499906c41e8caee8009
出典データセット
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03978056

反応ノート

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