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

HRID 1588047

반응식

HRID 1588047 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ec9c738cda3543fe863edba5cb923f72
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05220021

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