Sulfuric Acid → HCID 68707356, 화합물

HRID 645490노트

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HRID 645490 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].OS(O)(=O)=O.[ClH:12].[CH3:13][N:14]1[CH2:19][CH2:18][C:17]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)([C:20]#[N:21])[CH2:16][CH2:15]1>C1COCC1>[ClH:12].[ClH:12].[CH3:13][N:14]1[CH2:19][CH2:18][C:17]([CH2:20][NH2:21])([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:16][CH2:15]1

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 21226445Aluminium lithium hydrideHCID 248859601-Methyl-4-phenylpiperidine-4-carbonitrile--hydrogen chloride (1/1)

생성물 1

HCID 68707356HCID 68707356, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

To a solution of LAH (7.5 mmol) in THF (10 mL) is added dropwise conc. H2SO4 (3.8 mmol) at 0° C. After stirred at 0° C. for 0.5 h, 1-methyl-4-phenylpiperidine-4-carbonitrile hydrochloride (2.5 mmol) is added at 0° C. The reaction mixture is stirred at 60° C. for 6 h. After cooled down to 0° C., the reaction is quenched by the addition of Na2SO4-10H2O. The resulting mixture is filtered through celite, and the filtrate is concentrated in vacuo. The residue is suspended in ether and treated with HCl in 1,4-dioxane. The resulting white solid is collected by filtration to give the title compound, which is directly used for the next reaction without further purification.

후처리

  1. stirringThe reaction mixture is stirred at 60° C. for 6 h
  2. temperatureAfter cooled down to 0° C.
  3. customthe reaction is quenched by the addition of Na2SO4-10H2O
  4. filtrationThe resulting mixture is filtered through celite
  5. concentrationthe filtrate is concentrated in vacuo
  6. additiontreated with HCl in 1,4-dioxane
  7. filtrationThe resulting white solid is collected by filtration

출처 및 근거

ORD 기록
ord-7317d27a5b354a7994047732e0940f02
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07704996B2

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