1,2-Dichlorobenzene → HCID 18995918, 화합물

HRID 1108949노트

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HRID 1108949 반응식
[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

참가 물질

6

반응물 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

생성물 1

HCID 18995918HCID 18995918, 화합물수율 43.3%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
140 °C

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-1e2f31687c2645138810dce7cd8864bc
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05318959

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