Toluene → N-[2-(2-methyl-5-nitro-1-imidazolyl)ethyl]-3-nitrophthalimide

HRID 1973446

반응식

HRID 1973446 반응식
[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]2[C:7]([NH:9][C:10](=[O:11])[C:5]=12)=[O:8])([O-:3])=[O:2].[K].Cl[CH2:17][CH2:18][N:19]1[C:23]([N+:24]([O-:26])=[O:25])=[CH:22][N:21]=[C:20]1[CH3:27].C1(C)C=CC=CC=1>C(Cl)(Cl)Cl>[CH3:27][C:20]1[N:19]([CH2:18][CH2:17][N:9]2[C:10](=[O:11])[C:5]3=[C:4]([N+:1]([O-:3])=[O:2])[CH:14]=[CH:13][CH:12]=[C:6]3[C:7]2=[O:8])[C:23]([N+:24]([O-:26])=[O:25])=[CH:22][N:21]=1

참가 물질

6

반응물 4

HCID 1140TolueneHCID 117793-NitrophthalimideHCID 832101-(2-Chloroethyl)-2-methyl-5-nitroimidazoleHCID 5462222Potassium

생성물 1

HCID 21491667N-[2-(2-methyl-5-nitro-1-imidazolyl)ethyl]-3-nitrophthalimide

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

3-Nitrophthalimide is converted to the potassium salt by the procedure described in Example 13 and then reacted with 1-(2-chloroethyl)-2-methyl-5-nitroimidazole according to the procedure described in Example 1. The crude reaction mixture is digested with toluene and then filtered to remove some insoluble material. Evaporation of the solvent leaves a syrup which is diluted with chloroform and then filtered to remove some insoluble material. The filtrate is further diluted with toluene and again filtered to remove some precipitate. The solvent is then evaporated from the filtrate and the resulting residue is recrystallized first from ethanol and then from acetone to give N-[2-(2-methyl-5-nitro-1-imidazolyl)ethyl]-3-nitrophthalimide melting at about 175°-176° C.

후처리

  1. customThe crude reaction mixture
  2. filtrationfiltered
  3. customto remove some insoluble material
  4. customEvaporation of the solvent
  5. customleaves a syrup which
  6. filtrationfiltered
  7. customto remove some insoluble material
  8. additionThe filtrate is further diluted with toluene
  9. filtrationagain filtered
  10. customto remove some precipitate
  11. customThe solvent is then evaporated from the filtrate
  12. customthe resulting residue is recrystallized first from ethanol

출처 및 근거

ORD 기록
ord-dc05d02bf81342b9a9572f3970f7d9fb
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03997572

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