Sulfuric Acid → HCID 68707356、化合物

HRID 645490ノート

反応式

HRID 645490 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 68707356HCID 68707356、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7317d27a5b354a7994047732e0940f02
出典データセット
uspto-grants-2010_04
特許番号
US07704996B2

反応ノート

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