Triacetoxyperiodinane → 3-(3,4-Dichlorophenyl)-2-propynal

HRID 639842

반응식

HRID 639842 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]#[C:10][CH2:11][OH:12])[CH:5]=[CH:6][C:7]=1[Cl:8].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.C([O-])(O)=O.[Na+]>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]#[C:10][CH:11]=[O:12])[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

5

반응물 3

HCID 159087TriacetoxyperiodinaneHCID 516892Sodium BicarbonateHCID 230063813-(3,4-Dichlorophenyl)prop-2-yn-1-ol

생성물 1

HCID 592560003-(3,4-Dichlorophenyl)-2-propynal수율 98.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-(3,4-dichlorophenyl)-2-propyn-1-ol (2.980 g, P7, from Method A and B described for P7) in dry DCM (74 mL) and Dess-Martin periodinane (9.43 g) was added. The mixture was stirred at room temperature over night. NaS2O3 (19 g) and NaHCO3 saturated solution were then added to the mixture and it was stirred at room temperature for 1 hour. Then the organic phase was separated and washed with brine. The organic layer was dried and concentrated under reduced pressure to give the crude title product (2.9 g) that was used without further purification.

후처리

  1. stirringwas stirred at room temperature for 1 hour
  2. customThen the organic phase was separated
  3. washwashed with brine
  4. customThe organic layer was dried
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4086aa00965149cabd01a9265e66cd0d
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691893B2

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