Ammonium Chloride → Benzenemethanol, alpha-1-propen-1-yl-

HRID 913217

반응식

HRID 913217 반응식
[C:1]1([Mg]Br)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:9](=[O:13])/[CH:10]=[CH:11]/[CH3:12].[Cl-].[NH4+]>O1CCCC1.CCOCC>[C:1]1([CH:9]([OH:13])[CH:10]=[CH:11][CH3:12])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 447466CrotonaldehydeHCID 178418255HCID 178418255, 화합물

생성물 1

HCID 219674Benzenemethanol, alpha-1-propen-1-yl-수율 99.9%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

To a cooled (0-55° C.) 927 mL of 1 M solution of phenyl magnesium bromide in tetrahydofuran was added dropwise a solution of crotonaldehyde (65.0 g) in 130 mL of anhydrous ether over a period of 2 hours and 45 minutes. The reaction was stirred for an additional 45 minutes and then warmed to room temperature. After four more hours of stirring, saturated ammonium chloride aqueous solution (750 mL) was added to the reaction. The mixture was extracted with 750 mL of ether twice. The combined extract was dried over anhydrous potassium carbonate and filtered. The solvent was evaporated to give 135.88 g (99.9%) of the desired 1-phenyl-2-buten-1-ol as an oil which was used in the next step without further purification.

후처리

  1. custom45 minutes
  2. stirringAfter four more hours of stirring
  3. extractionThe mixture was extracted with 750 mL of ether twice
  4. extractionThe combined extract
  5. dry with materialwas dried over anhydrous potassium carbonate
  6. filtrationfiltered
  7. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-f7a6682c212e4a11bbfe582263c29537
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026280B2

연결된 노트

불러오는 중…