1,2-Dichlorobenzene → HCID 18995918、化合物

HRID 1108949ノート

反応式

HRID 1108949 の反応式
[CH3:1][N:2](S(C1C=CC=CC=1)(=O)=O)[N:3]=[C:4](Cl)[C:5]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:12].[Cl:23][C:24]1[C:25]([O:34][C:35]2[CH:42]=[CH:41][C:38]([C:39]#[N:40])=[CH:37][CH:36]=2)=[N:26][CH:27]=[C:28]([C:30]([F:33])([F:32])[F:31])[CH:29]=1.[Cl-].[Al+3].[Cl-].[Cl-].ClC1C=CC=CC=1Cl>C(Cl)(Cl)Cl>[Cl:12][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]([F:11])[C:5]=1[C:4]1[N:40]=[C:39]([C:38]2[CH:37]=[CH:36][C:35]([O:34][C:25]3[C:24]([Cl:23])=[CH:29][C:28]([C:30]([F:33])([F:31])[F:32])=[CH:27][N:26]=3)=[CH:42][CH:41]=2)[N:2]([CH3:1])[N:3]=1

参加物

6

反応物 4

HCID 72391,2-DichlorobenzeneHCID 27444784-((3-Chloro-5-(trifluoromethyl)pyridin-2-yl)oxy)benzonitrileHCID 6451240Aluminum(III) ChlorideHCID 53760501N-methyl-N-phenylsulfonyl-2-chloro-6-fluorobenzohydrazonoyl chloride

生成物 1

HCID 18995918HCID 18995918、化合物収率 43.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
140 °C

実験手順

A mixture of 1.30 g of N-methyl-N-phenylsulfonyl-2-chloro-6-fluorobenzohydrazonoyl chloride, 1.00 g of 4-(3-chloro-5-trifluoromethylpyridin-2-yloxy)benzonitrile, 0.50 g of anhydrous aluminum chloride and 3 ml of o-dichlorobenzene was stirred in an oil bath at a temperature of 140° C. for 30 minutes. After the cooling, the resulting solution was dissolved in 100 ml of chloroform, washed with diluted hydrochloric acid solution, diluted sodium hydroxide solution and saline water in this order, dried over anhydrous magnesium sulfate and concentrated under a reduced pressure. The resulting concentrate was purified through a chromatography of silica gel column using a mixed solution of hexane and ethyl acetate as a developing solvent to obtain 0.70 g of the given compound (measurement of nD20 was impossible). NMR data (60 MHz, CDCl3 solvent, δ value)

後処理

  1. washwashed with diluted hydrochloric acid solution, diluted sodium hydroxide solution and saline water in this order
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under a reduced pressure
  4. concentrationThe resulting concentrate
  5. customwas purified through a chromatography of silica gel column

出典と根拠

ORDレコード
ord-1e2f31687c2645138810dce7cd8864bc
出典データセット
uspto-grants-1994_06
特許番号
US05318959

反応ノート

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