Carbon Tetrachloride → HCID 13854292, 화합물

HRID 1200073노트

반응식

HRID 1200073 반응식
[CH3:1][C:2]([CH3:21])([CH2:5][O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:9]=1)[CH:3]=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:41](Cl)(Cl)([Cl:43])[Cl:42]>[Zn]>[CH3:1][C:2]([CH3:21])([CH:3]=[C:41]([Cl:43])[Cl:42])[CH2:5][O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:9]=1

참가 물질

5

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 138494092,2-Dimethyl-3-[(3-phenoxyphenyl)methoxy]propanal

생성물 1

HCID 13854292HCID 13854292, 화합물

시약·촉매·용매 1

HCID 23994Zinc촉매

실험 절차

A mixture of 2,2-dimethyl-3-(3-phenoxybenzyloxy)propan-1-al (0.25 g), triphenylphosphine (0.47 g), zinc dust (0.12 g) and carbon tetrachloride (0.2 cm3) was heated at the relux temperature for one hour. After cooling to the ambient temperature (ca 25° C.) the mixture was diluted with petroleum ether (boiling range 40°-60° C.) and the solid component removed by filtration. The filtrate was concentrated by evaporation of the solvent under reduced pressure, and the residual oil subjected to purification by flash chromatography using a silica gel column eluted with dichloromethane to yield 2,2-dimethyl-1-(3-phenoxybenzyloxy)-4,4-dichlorobut-3-ene (0.2 g).

후처리

  1. temperaturewas heated at the relux temperature for one hour
  2. customthe solid component removed by filtration
  3. concentrationThe filtrate was concentrated by evaporation of the solvent under reduced pressure
  4. customthe residual oil subjected to purification by flash chromatography
  5. washeluted with dichloromethane

출처 및 근거

ORD 기록
ord-188cb210b25e437295039a1e7648a536
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04904677

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