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Water → HCID 19928725, 화합물

HRID 1974898
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HRID 1974898 반응식
[CH3:1][NH:2][CH:3]([C:6]([CH3:19])([OH:18])[CH2:7][CH2:8][CH2:9][CH:10]([CH3:17])[CH2:11][CH2:12][CH2:13][CH:14]([CH3:16])[CH3:15])[CH2:4][OH:5].N1C=CC=CC=1.Cl.[C:27](Cl)(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[N:30][CH:29]=1.O>ClC(Cl)C>[CH3:1][N:2]([CH:3]([C:6]([OH:18])([CH3:19])[CH2:7][CH2:8][CH2:9][CH:10]([CH3:17])[CH2:11][CH2:12][CH2:13][CH:14]([CH3:15])[CH3:16])[CH2:4][OH:5])[C:27](=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[N:30][CH:29]=1
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6

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HCID 962WaterHCID 1049PyridineHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 199287142-(N-Methylamino)-3,7,11-trimethyl-1,3-dodecanediol

생성물 1

HCID 19928725HCID 19928725, 화합물

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

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온도
-30 °C

실험 절차

In 100 ml of dichloroethane were dissolved 10 g of 2-(methylamino)-3,7,11-trimethyl-1,3-dodecanediol and 8.7 g of pyridine and the solution was cooled to -30° C. To this solution was added 7.2 g of nicotinoyl chloride hydrochloride gradually and the mixture was stirred at room temperature for 3 hours. After the reaction was completed, the reaction mixture was poured into water and extracted with dichloroethane. The organic layer was washed with aqueous sodium hydrogen carbonate and after drying over anhydrous magnesium sulfate, the solvent was distilled off. Finally, the residue was subjected to silica gel column chromatography (elution with ethanol) to give 12.0 q of N-methyl-N-(1,3-dihydroxy-3,7,11-trimethyldodecan-2-yl)nicotinamide [Compound (66)]. Yield 93%.

후처리

  1. extractionextracted with dichloroethane
  2. washThe organic layer was washed with aqueous sodium hydrogen carbonate
  3. dry with materialafter drying over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off
  5. washFinally, the residue was subjected to silica gel column chromatography (elution with ethanol)

출처 및 근거

ORD 기록
ord-560715144dd14ad8a8825814d1ca038c
출처 데이터셋
uspto-grants-1994_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05284850

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