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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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1,2-Dichlorobenzene → 5-(4-chloro-3-octyloxyphenyl)-3-(2-chlorophenyl) 1-methyl-1H-1,2,4-triazole

HRID 1940714
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HRID 1940714 반응식
[CH3:1][N:2](S(C1C=CC=CC=1)(=O)=O)[N:3]=[C:4](Cl)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:11].[Cl:22][C:23]1[CH:30]=[CH:29][C:26]([C:27]#[N:28])=[CH:25][C:24]=1[O:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39].ClC1C=CC=CC=1Cl>C(Cl)(Cl)Cl.[Fe](Cl)(Cl)Cl>[Cl:22][C:23]1[CH:30]=[CH:29][C:26]([C:27]2[N:2]([CH3:1])[N:3]=[C:4]([C:5]3[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=3[Cl:11])[N:28]=2)=[CH:25][C:24]=1[O:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39]
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참가 물질

6

반응물 3

HCID 72391,2-DichlorobenzeneHCID 214636694-Chloro-3-octyloxybenzonitrileHCID 54508988N-methyl-N-phenylsulfonyl-2-chlorobenzohydrazonoyl chloride

생성물 1

HCID 214636325-(4-chloro-3-octyloxyphenyl)-3-(2-chlorophenyl) 1-methyl-1H-1,2,4-triazole수율 42.3%

시약·촉매·용매 2

HCID 24380Iron chloride (FeCl3)촉매
HCID 6212
Chloroform
용매

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온도
140 °C

실험 절차

A mixture of N-methyl-N-(benzenesulfonyl)-2-chlorobenzohydrazonoyl chloride (1.50 g), 4-chloro-3-octyloxybenzonitrile (1.30 g), anhydrous iron (III) chloride (0.80 g) and o-dichlorobenzene (5 ml) is stirred at an oil bath temperature of 140° C. for 30 minutes. After cooling, the reaction mixture is dissolved in chloroform (100 ml), washed with dilute hydrochloric acid, dilute aqueous solution of sodium hydroxide and saline in this order, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography using mixed solvent of hexane-ethyl acetate as eluent to give 0.80 g of desired compound.

후처리

  1. temperatureAfter cooling
  2. washwashed with dilute hydrochloric acid, dilute aqueous solution of sodium hydroxide and saline in this order
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe concentrate is purified by silica gel column chromatography
  6. additionusing mixed solvent of hexane-ethyl acetate as eluent

출처 및 근거

ORD 기록
ord-1ec6a5726f3a484da1352c94937642b4
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05700824

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