4-Methylmorpholine → HCID 59140422, 화합물

HRID 1927667노트

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HRID 1927667 반응식
CN1CCOCC1.[CH3:8][C:9]([CH3:18])([CH2:16][CH3:17])[CH2:10][C:11]1[N:12]=[CH:13][NH:14][CH:15]=1.[CH3:19][N:20]([CH3:25])[S:21](Cl)(=[O:23])=[O:22]>C(COC)OC>[CH3:8][C:9]([CH3:18])([CH2:16][CH3:17])[CH2:10][C:11]1[N:12]=[CH:13][N:14]([S:21]([N:20]([CH3:25])[CH3:19])(=[O:23])=[O:22])[CH:15]=1

참가 물질

5

반응물 3

HCID 79724-Methylmorpholine2회HCID 83372Dimethylsulphamoyl chloride2회HCID 178442466HCID 178442466, 화합물

생성물 1

HCID 59140422HCID 59140422, 화합물

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

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온도
40 °C

실험 절차

N-Methylmorpholine (54 mL, 0.48 mol) was added to a solution of 4-(2,2-dimethylbutyl)-1H-imidazole (36 g, 0.24 mol) in dimethoxyethane (360 mL). After warming to 40° C., N,N-dimethylsulfamoyl chloride (38 mL, 0.36 mol) was added over 15 min. After stirring at 40° C. for 2 h, N-methylmorpholine (11 mL) and N,N-dimethylsulfamoyl chloride (8 mL) were added. After stirring for additional 2 h, the reaction mixture was cooled and filtered rinsing with ether. The filtrate was extracted with ether and the combined extracts were washed with brine, dried (magnesium sulfate), filtered, concentrated in vacuo. Chromatography over silica gel afforded the title compound.

후처리

  1. stirringAfter stirring for additional 2 h
  2. temperaturethe reaction mixture was cooled
  3. filtrationfiltered
  4. washrinsing with ether
  5. extractionThe filtrate was extracted with ether
  6. washthe combined extracts were washed with brine
  7. dry with materialdried (magnesium sulfate)
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-68b2f512f0914ff1b09e631d98235bd5
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183275B2

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