Hydrochloric Acid → 3-Ethynylbenzonitrile

HRID 606787

반응식

HRID 606787 반응식
C(=O)([O-])[O-].[K+].[K+].C[Si]([C:11]#[C:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[C:16]#[N:17])(C)C.Cl>CO>[C:12]([C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[C:16]#[N:17])#[CH:11]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 225703183-[(Trimethylsilyl)ethynyl]benzonitrile

생성물 1

HCID 120889643-Ethynylbenzonitrile수율 92%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Add potassium carbonate (0.138 g, 1 mmol) to a solution of 3-trimethylsilanylethynylbenzonitrile from PREPARATION 5 (2.0 g, 10.1 mmol) in methanol (50 mL). Stir the mixture at room temperature for 20 min and add a 10% aqueous hydrochloric acid solution (4 mL). Concentrate to a reduced volume, add diethyl ether and water and separate the phases. Wash once the aqueous phase with diethyl ether. Combine the organic phases, dry over sodium sulfate and concentrate to obtain the title compound as a solid (1.17 g, 92%).

후처리

  1. concentrationConcentrate to a reduced volume
  2. additionadd diethyl ether and water
  3. customseparate the phases
  4. washWash once the aqueous phase with diethyl ether
  5. dry with materialdry over sodium sulfate
  6. concentrationconcentrate

출처 및 근거

ORD 기록
ord-0eabd544b1254993971a164e6b861429
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915424B2

연결된 노트

불러오는 중…