Water → HCID 816842、化合物

HRID 2041572ノート

反応式

HRID 2041572 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 816842HCID 816842、化合物収率 97.9%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒

反応条件

温度
0 °C

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-e0f07cfe6c4248cc861065db9bc0b51d
出典データセット
uspto-grants-2013_11
特許番号
US08580780B2

反応ノート

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