1,2-Dichlorobenzene → HCID 19021367, 화합물

HRID 1108948노트

반응식

HRID 1108948 반응식
[CH3:1][N:2](S(C1C=CC=CC=1)(=O)=O)[N:3]=[C:4](Cl)[C:5]1[C:10]([Cl:11])=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:12].[CH2:23]([O:33][C:34]1[CH:41]=[CH:40][C:37]([C:38]#[N:39])=[CH:36][CH:35]=1)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32].[Cl-].[Al+3].[Cl-].[Cl-].ClC1C=CC=CC=1Cl>C(Cl)(Cl)Cl>[CH2:23]([O:33][C:34]1[CH:41]=[CH:40][C:37]([C:38]2[N:2]([CH3:1])[N:3]=[C:4]([C:5]3[C:6]([Cl:12])=[CH:7][CH:8]=[CH:9][C:10]=3[Cl:11])[N:39]=2)=[CH:36][CH:35]=1)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32]

참가 물질

6

반응물 4

HCID 72391,2-DichlorobenzeneHCID 6451240Aluminum(III) ChlorideHCID 190213714-(Decyloxy)benzonitrileHCID 54261612HCID 54261612, 화합물

생성물 1

HCID 19021367HCID 19021367, 화합물수율 32.2%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
140 °C

실험 절차

A mixture of 1.10 g of N-methyl-N-phenylsulfonyl-2,6-dichlorobenzohydrazonoyl chloride, 0.70 g of 4-decyloxybenzonitrile, 0.4 g of anhydrous aluminium 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 0.40 g of the given compound (melting point: 60.0°-64.0° C.).

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-b00c3026da4247f0978f845febb022a9
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05318959

반응 노트

불러오는 중…