Water → HCID 816842, 화합물

HRID 2041572노트

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HRID 2041572 반응식
[C:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1)#[N:2].[Cl-].[Cl-].[Cl-].[Al+3].O>C1(C)C=CC=CC=1.C(OCC)C>[CH3:1][C:3]1[CH:11]=[CH:10][C:6]([C:7]([C:6]2[CH:10]=[CH:11][C:3]([C:1]#[N:2])=[CH:4][CH:5]=2)=[O:8])=[CH:5][CH:4]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 801724-Cyanobenzoyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 816842HCID 816842, 화합물수율 97.9%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매

반응 조건

온도
0 °C

실험 절차

Suspend 4-cyanobenzoyl chloride (2.0 g, 12 mmol) in anhydrous toluene (30 mL). Add aluminum trichloride (2.4 g, 18 mmol) in three portions and stir the reaction mixture at ambient temperature overnight. Cool to 0° C., add carefully water and extract the mixture twice with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo to give a solid. Suspend the solid in diethyl ether and filter to obtain the desired intermediate (1.30 g, 49%) that was used without any further purification. GC-MS m/z: 221 (M+).

후처리

  1. extractionextract the mixture twice with EtOAc
  2. dry with materialDry the combined organic extracts over Na2SO4
  3. filtrationfilter
  4. concentrationconcentrate in vacuo
  5. customto give a solid
  6. filtrationfilter

출처 및 근거

ORD 기록
ord-e0f07cfe6c4248cc861065db9bc0b51d
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08580780B2

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