Water → 5-(2,2,2-Trifluoro-1-(trifluoromethyl)ethyl)-2-methoxybenzaldehyde

HRID 2269244노트

반응식

HRID 2269244 반응식
[F:1][C:2]([F:17])([F:16])[CH:3]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1)[C:4]([F:7])([F:6])[F:5].[CH:18]([O:21]C)(Cl)Cl.O>C(Cl)Cl.Cl[Ti](Cl)(Cl)Cl>[F:1][C:2]([F:16])([F:17])[CH:3]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([CH:9]=1)[CH:18]=[O:21])[C:4]([F:6])([F:5])[F:7]

참가 물질

6

반응물 3

HCID 962WaterHCID 21004Methane, dichloromethoxy-HCID 183336204-(2,2,2-Trifluoro-1-(trifluoromethyl)ethyl)anisole

생성물 1

HCID 186776145-(2,2,2-Trifluoro-1-(trifluoromethyl)ethyl)-2-methoxybenzaldehyde수율 90.9%

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 6344Dichloromethane용매

실험 절차

To a stirred and ice-cooled solution of Compound 8 (650 mg, 2.5 mmol) in dry CH2Cl2 (15 ml) was added neat TiCl4 (950 mg, 5.0 mmol) followed by Cl2CHOMe (600 mg, 5.0 mmol). After the addition was complete, the mixture was stirred at room temperature for 5 hr, poured into H2O (60 ml), and extracted with CH2Cl2. The combined extracts were dried (Na2SO4), and concentrated in vacuo to give a yellow oil, which was purified by a column chromatography on silica gel to give Compound 9 (650 mg, 90%)

후처리

  1. additionAfter the addition
  2. stirringthe mixture was stirred at room temperature for 5 hr
  3. extractionextracted with CH2Cl2
  4. dry with materialThe combined extracts were dried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customto give a yellow oil, which
  7. customwas purified by a column chromatography on silica gel

출처 및 근거

ORD 기록
ord-775882272a5847b1b8636a5059b798c2
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329396B1

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