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Water → 2-hydroxymethyl-4-isopropyl-1-(pyridin-4-yl)-1H-imidazole

HRID 8405
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인쇄 미리보기

반응식

HRID 8405 반응식
C([O:8][CH2:9][C:10]1[N:11]([C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)[CH:12]=[C:13]([CH:15]([CH3:17])[CH3:16])[N:14]=1)C1C=CC=CC=1.O.C1(C)C=CC=CC=1>Cl>[OH:8][CH2:9][C:10]1[N:11]([C:18]2[CH:19]=[CH:20][N:21]=[CH:22][CH:23]=2)[CH:12]=[C:13]([CH:15]([CH3:17])[CH3:16])[N:14]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 1140TolueneHCID 220157572-Benzyloxymethyl-4-isopropyl-1-(pyridin-4-yl)-1H-imidazole

생성물 1

HCID 220157552-hydroxymethyl-4-isopropyl-1-(pyridin-4-yl)-1H-imidazole수율 86.6%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
85 °C

실험 절차

The compound (5) (20.0 g, 62.2 mmol) was suspended in 35% aqueous hydrochloric acid (100 ml). The solution was heated at 85° C. and stirred for 1 hour. The reaction mixture was cooled down to room temperature and water (100 ml) and toluene (44 ml) were added thereto with stirring. The aqueous layer was separated and neutralized with 30% aqueous sodium hydroxide, to which ethyl acetate (30 ml) was added with stirring. The obtained slurry was filtered, washed with cold water and dried to yield 2-hydroxymethyl-4-isopropyl-1-(pyridin-4-yl)-1H-imidazole (9) (11.7 g). Yield 81.4%.

후처리

  1. temperatureThe reaction mixture was cooled down to room temperature
  2. stirringwith stirring
  3. customThe aqueous layer was separated
  4. additionwas added
  5. stirringwith stirring
  6. filtrationThe obtained slurry was filtered
  7. washwashed with cold water
  8. customdried

출처 및 근거

ORD 기록
ord-817f567d751f49859e698e37d51e69b5
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07087764B2

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