Water → 4-Methyl-1-nitro-2-[2-(2-nitrophenoxy)ethoxy]benzene

HRID 1852365노트

반응식

HRID 1852365 반응식
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N+:11]([O-:13])=[O:12].[CH3:14][C:15]1[CH:16]=[CH:17][C:18]([N+:22]([O-:24])=[O:23])=[C:19]([OH:21])[CH:20]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[CH3:14][C:15]1[CH:16]=[CH:17][C:18]([N+:22]([O-:24])=[O:23])=[C:19]([O:21][CH2:2][CH2:3][O:4][C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[N+:11]([O-:13])=[O:12])[CH:20]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 127886-Nitro-m-cresolHCID 43624871-(2-chloroethoxy)-2-nitrobenzene

생성물 1

HCID 27630554-Methyl-1-nitro-2-[2-(2-nitrophenoxy)ethoxy]benzene

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

1-(2-Chloro-ethoxy)-2-nitro-benzene (116 g) and 5-methyl-2-nitro-phenol (88 g) were dissolved in 500 ml DMF and was stirred for 4 h at 90-110° C. after careful addition of 160 g potassium carbonate. The reaction mixture was poured in a mixture of crushed ice and water (8 l) which was vigorously stirred. The residue was filtered off, washed several times with water and dried. The crude product was suspended in methanol and the pale yellow residue was again filtered off, washed with methanol and dried. Yield: 150-165 g.

후처리

  1. stirringwas vigorously stirred
  2. filtrationThe residue was filtered off
  3. washwashed several times with water
  4. customdried
  5. filtrationthe pale yellow residue was again filtered off
  6. washwashed with methanol
  7. customdried

출처 및 근거

ORD 기록
ord-22c6d06fd49b4326b2ec6360d3ecb503
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962338B2

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