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Hydrochloric Acid → HCID 22130877, 화합물

HRID 1857734
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HRID 1857734 반응식
C([O:8][CH2:9][C:10]1[N:11]([CH3:27])[C:12]([CH2:18][C:19]2[CH:24]=[C:23]([Cl:25])[CH:22]=[C:21]([Cl:26])[CH:20]=2)=[C:13]([CH:15]([CH3:17])[CH3:16])[N:14]=1)C1C=CC=CC=1.Cl>C(O)C>[Cl:26][C:21]1[CH:20]=[C:19]([CH:24]=[C:23]([Cl:25])[CH:22]=1)[CH2:18][C:12]1[N:11]([CH3:27])[C:10]([CH2:9][OH:8])=[N:14][C:13]=1[CH:15]([CH3:16])[CH3:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 22130078HCID 22130078, 화합물

생성물 1

HCID 22130877HCID 22130877, 화합물수율 95.9%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
110 °C

실험 절차

In 3 ml of ethanol was dissolved 470 mg (1.17 mmol) of 2-benzyloxymethyl-5-(3,5-dichlorobenzyl)-4-isopropyl-1-methyl-1H-imidazole (58), followed by addition of 10 ml of concentrated hydrochloric acid (36% aqueous solution), and the mixture was refluxed under heating at 110° C. After 3 hours, the reaction mixture was concentrated under reduced pressure, neutralized with aqueous sodium hydroxide, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated. To the crude crystals, 5 ml of diethyl ether was added, and filtered to give 350 mg of [5-(3,5-dichlorobenzyl)-4-isopropyl-1-methyl-1H-imidazol-2-yl]methanol (59a) (yield 95.9%).

후처리

  1. temperaturethe mixture was refluxed
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated
  8. additionTo the crude crystals, 5 ml of diethyl ether was added
  9. filtrationfiltered

출처 및 근거

ORD 기록
ord-268a47f2c1614fcb81f3cf5e314d73fe
출처 데이터셋
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06147097

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