4-Nitrobenzoyl chloride → Ethanone,2-diazo-(4-nitrophenyl)-

HRID 1588047ノート

反応式

HRID 1588047 の反応式
[N+:1](=[CH2:3])=[N-:2].CN(N=O)/C(/N)=N/[N+]([O-])=O.[OH-].[K+].[N+:16]([C:19]1[CH:27]=[CH:26][C:22]([C:23](Cl)=[O:24])=[CH:21][CH:20]=1)([O-:18])=[O:17]>CCOCC>[N+:1](=[CH:3][C:23]([C:22]1[CH:21]=[CH:20][C:19]([N+:16]([O-:18])=[O:17])=[CH:27][CH:26]=1)=[O:24])=[N-:2]

参加物

6

反応物 4

HCID 85024-Nitrobenzoyl chlorideHCID 9550DiazomethaneHCID 14797Potassium HydroxideHCID 95620601-Methyl-2-nitro-1-nitrosoguanidine

生成物 1

HCID 138152Ethanone,2-diazo-(4-nitrophenyl)-

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

The ethereal diazomethane solution [prepared by adding 12.5 g n-methyl-n-nitro-n-nitroso guanidine to potassium hydroxide (50%, 20 ml) and ether (200 ml) at 0°, stirring for 1 hr, and decanting the ether layer; 65% presumed yield] is treated with TEA (7.7 ml) at 0°, then dropwise with p-nitrobenzoyl chloride (10.21 ml) in ether (25 ml). After stirring for 19 hrs, the reaction is filtered through celite and concentrated to give the title compound.

後処理

  1. customdecanting the ether layer
  2. custom65% presumed yield]
  3. stirringAfter stirring for 19 hrs
  4. filtrationthe reaction is filtered through celite and
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-ec9c738cda3543fe863edba5cb923f72
出典データセット
uspto-grants-1993_06
特許番号
US05220021

反応ノート

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