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

HRID 1886980ノート

反応式

HRID 1886980 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-493ff34e60c14238a601e5d8499ab7f5
出典データセット
uspto-grants-2013_08
特許番号
US08501727B2

反応ノート

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