Ethyl Acetate → 2-Chloro-4-methylbenzonitrile

HRID 1172674

반응식

HRID 1172674 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[Cl:9].[Cu][C:11]#[N:12].C(OCC)(=O)C>CN(C)C=O>[Cl:9][C:3]1[CH:4]=[C:5]([CH3:8])[CH:6]=[CH:7][C:2]=1[C:11]#[N:12]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 1387894-Bromo-3-chlorotolueneHCID 178418546HCID 178418546, 화합물

생성물 1

HCID 3194752-Chloro-4-methylbenzonitrile수율 93.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

25.0 g 4-bromo-3-chlorotoluene and 21.8 g copper (I) cyanide were dissolved in 200 ml dimethylformamide and stirred at 150° C. for three hours. The cooled reaction mixture was diluted by addition of 300 ml ethyl acetate and washed three times with portions of 150 ml saturated NH4Cl solution. The precipitates were filtered off and the filtrate dried over MgSO4 and then reduced in vacuo to obtain 17.3 g 2-Chloro-4-methyl-benzonitrile. This material was used without purification in the next step.

후처리

  1. customThe cooled reaction mixture
  2. washwashed three times with portions of 150 ml saturated NH4Cl solution
  3. filtrationThe precipitates were filtered off
  4. dry with materialthe filtrate dried over MgSO4

출처 및 근거

ORD 기록
ord-7d56b42e5602451ba9f5a80875b098d2
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834030B2

연결된 노트

불러오는 중…