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

HRID 727849ノート

反応式

HRID 727849 の反応式
[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

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 145143764-[1-(1-Imidazolyl)-butyl]-benzyl alcoholHCID 178418573HCID 178418573、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

  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))

出典と根拠

ORDレコード
ord-a773e42e0ebb4870bcd6bbe0cf1d3915
出典データセット
uspto-grants-1991_09
特許番号
US05045558

反応ノート

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