Hydrochloric Acid → 1-[4-[1-(1-Imidazolyl)-butyl]-phenyl]-ethanol

HRID 727849노트

반응식

HRID 727849 반응식
[N:1]1([CH:6]([C:10]2[CH:17]=[CH:16][C:13]([CH2:14][OH:15])=[CH:12][CH:11]=2)[CH2:7][CH2:8][CH3:9])[CH:5]=[CH:4][N:3]=[CH:2]1.[CH3:18][Mg]Br.O1CCCC1.Cl>CCOCC>[N:1]1([CH:6]([C:10]2[CH:11]=[CH:12][C:13]([CH:14]([OH:15])[CH3:18])=[CH:16][CH:17]=2)[CH2:7][CH2:8][CH3:9])[CH:5]=[CH:4][N:3]=[CH:2]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 145143764-[1-(1-Imidazolyl)-butyl]-benzyl alcoholHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 198251771-[4-[1-(1-Imidazolyl)-butyl]-phenyl]-ethanol

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

460 mg of the aldehyde of example 5 in 8 ml of ether is mixed with 1.5 ml of a 3M methyl magnesium bromide solution in ether with ice cooling and is stirred for 20 hours at room temperature; 10 ml of tetrahydrofuran is added and heated to 60° C. in 6 hours. It is added to 1M of hydrochloric acid, extracted with ether, then the water phase is alkalized with potassium carbonate and extracted with ether. After drying and concentration by evaporation of this ether phase, the residue is chromatographed on silica gel (methylene chloride/methanol (95:5)). 300 mg of the title compound is obtained.

후처리

  1. temperatureheated to 60° C. in 6 hours
  2. extractionextracted with ether
  3. extractionextracted with ether
  4. customAfter drying
  5. concentrationconcentration
  6. customby evaporation of this ether phase
  7. customthe residue is chromatographed on silica gel (methylene chloride/methanol (95:5))

출처 및 근거

ORD 기록
ord-a773e42e0ebb4870bcd6bbe0cf1d3915
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05045558

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