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Hydrochloric Acid → Dodecylamine

HRID 8100
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HRID 8100 반응식
C(OC(=O)N[C:8]([CH3:29])(C)[CH2:9][C:10]1[C:18]2[C:13](=[C:14](OC3C(C#N)=CC=CN=3)[CH:15]=[CH:16][CH:17]=2)[NH:12]C=1)(C)(C)C.Cl.O1CCO[CH2:34][CH2:33]1>>[CH3:33][CH2:34][CH2:29][CH2:8][CH2:9][CH2:10][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][NH2:12]
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참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-Dioxane2회HCID 69516986{2-[7-(3-cyano-pyridin-2-yloxy)-1H-indol-3-yl]-1,1-dimethyl-ethyl}-carbamic acid tert-butyl ester

생성물 1

HCID 13583Dodecylamine수율 83%

실험 절차

{2-[7-(3-Cyano-pyridin-2-yloxy)-1H-indol-3-yl]-1,1-dimethyl-ethyl}-carbamic acid tert-butyl ester (119 mg, 0.293 mmol) is dissolved in 10 mL of 1,4 dioxane. The mixture is cooled to zero degrees Celsius in an ice/water bath. To the mixture is added 10 mL of 4N hydrochloric acid in 1,4 dioxane, and the resulting mixture is stirred at zero degrees, under nitrogen, for five hours. The solvent is evaporated, and the residue is taken up in water. The pH of the water is adjusted to 9 using sodium bicarbonate, and is extracted three times with 50 mL of ethyl acetate. The organic layers are combined, dried with sodium sulfate, filtered, and the solvent removed in vacuo to give 218 mg of the title amine (83%). FDMS m/e=307 (M++1).

후처리

  1. temperatureThe mixture is cooled to zero degrees Celsius in an ice/water bath
  2. customThe solvent is evaporated
  3. extractionis extracted three times with 50 mL of ethyl acetate
  4. dry with materialdried with sodium sulfate
  5. filtrationfiltered
  6. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-738a85bc0da5412e8b8a396e20525741
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07087635B2

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