Water → 1-(Benzyloxy)-2-chloro-3-nitrobenzene

HRID 1886980노트

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HRID 1886980 반응식
[Cl:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:11].C(=O)([O-])[O-].[Cs+].[Cs+].[CH2:18](Br)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.O>CN(C)C=O>[CH2:18]([O:11][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([N+:8]([O-:10])=[O:9])[C:2]=1[Cl:1])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 7498Benzyl BromideHCID 10796Cesium carbonateHCID 3013917Phenol, 2-chloro-3-nitro-

생성물 1

HCID 143561211-(Benzyloxy)-2-chloro-3-nitrobenzene

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

A mixture of 5.37 g (30.9 mmol) of 2-chloro-3-nitrophenol and 12.6 g (38.7 mmol) of cesium carbonate in 60 mL of dimethylformamide (DMF) was cooled to 0° C. and 4.04 mL (34.0 mmol) of benzyl bromide was added. The mixture was warmed to 22° C. and stirred for 16 hours. Water was added and the resulting mixture was extracted with ether. The organic extract was dried (Na2SO4) and evaporated. The residue was crystallized from ethyl acetate and hexane to give 1-(benzyloxy)-2-chloro-3-nitrobenzene.

후처리

  1. temperatureThe mixture was warmed to 22° C.
  2. extractionthe resulting mixture was extracted with ether
  3. extractionThe organic extract
  4. dry with materialwas dried (Na2SO4)
  5. customevaporated
  6. customThe residue was crystallized from ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-493ff34e60c14238a601e5d8499ab7f5
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501727B2

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