Potassium Hydroxide → HCID 20131160, 화합물

HRID 1380113노트

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HRID 1380113 반응식
[OH:1][CH:2]([CH2:9][O:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=1)[CH2:3][N:4]1[CH:8]=[CH:7][N:6]=[CH:5]1.[OH-].[K+].Br[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]([O:30][CH:31]([CH3:33])[CH3:32])=[O:29].[Cl-].[NH4+]>CS(C)=O>[N:4]1([CH2:3][CH:2]([CH2:9][O:10][CH2:11][C:12]2[CH:13]=[CH:14][C:15]([O:18][CH3:19])=[CH:16][CH:17]=2)[O:1][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][C:28]([O:30][CH:31]([CH3:32])[CH3:33])=[O:29])[CH:8]=[CH:7][N:6]=[CH:5]1

참가 물질

6

반응물 4

HCID 14797Potassium HydroxideHCID 25517Ammonium ChlorideHCID 549816Isopropyl 6-bromohexanoateHCID 13590265HCID 13590265, 화합물

생성물 1

HCID 20131160HCID 20131160, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

1-[2-Hydroxy-3-[(4-methoxyphenyl)methoxy]propyl]-1H-imidazole (Example 1b; 10 g, 0.038 mol) was added to a stirred suspension of powdered potassium hydroxide (8 g, 0.14 mol) in dimethylsulphoxide (20 ml) at 18° C. and stirred for 0.5 hours. Isopropyl 6-bromohexanoate (10.5 g, 0.044 mol) was then added and the mixture was stirred for 0.5 hours at 18° C. The mixture was poured into saturated aqueous ammonium chloride (1500 ml) and extracted with dichloromethane. The combined extracts were dried (Na2SO4) and the solvent was evaporated off under reduced pressure to give the crude product which was purified by column chromatography (silica gel, 2% ethanol in chloroform) to give isopropyl 6-[2-(1H-imidazol-1-yl)-1-[[(4-methoxyphenyl)methoxy]methyl]ethoxy]hexanoate as a pale-yellow oil.

후처리

  1. stirringthe mixture was stirred for 0.5 hours at 18° C
  2. extractionextracted with dichloromethane
  3. dry with materialThe combined extracts were dried (Na2SO4)
  4. customthe solvent was evaporated off under reduced pressure
  5. customto give the crude product which
  6. customwas purified by column chromatography (silica gel, 2% ethanol in chloroform)

출처 및 근거

ORD 기록
ord-b73c89241d3841f9b687a95d2adf7234
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04579862

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