Potassium Hydroxide → 1,3-Dichloro-5-ethynylbenzene

HRID 24011노트

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HRID 24011 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]#[C:10][Si](C)(C)C)[CH:5]=[C:6]([Cl:8])[CH:7]=1.[OH-].[K+]>CO.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]#[CH:10])[CH:5]=[C:6]([Cl:8])[CH:7]=1

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 22570337[2-(3,5-Dichlorophenyl)ethynyl]trimethylsilane

생성물 1

HCID 138235471,3-Dichloro-5-ethynylbenzene수율 87.3%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

실험 절차

To a solution of (3,5-dichloro-phenylethynyl)-trimethyl-silane (1.97 g, 8.1 mmol) in methanol (40 mL) was added a solution of potassium hydroxide (6.8 mg, 0.12 mmol) in H2O (0.24 mL). After stirring at ambient temperature for 40 minutes, the reaction mixture was diluted with water (40 mL), and extracted with hexane until the extracting solvent showing no product by TLC. The combined organic layer was dried over MgSO4, and concentrated to give the title compound (1.21 g, 87% yield) as a white solid. 1H NMR (CDCl3) δ 7.37-7.34 (m, 3H), 3.15 (s, 1H).

후처리

  1. extractionextracted with hexane until the extracting solvent
  2. dry with materialThe combined organic layer was dried over MgSO4
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-330c0c3ee0b143eea7324012c8728a63
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06855722B2

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