Acetate → 6-acetylamino-1-(3-methylbenzyl)-4-methylhexahydro-1H-1,4-diazepine

HRID 374111

反応式

HRID 374111 の反応式
C([O-])(=O)C.[C:5]([NH:8][CH:9]1[CH2:15][N:14]([CH3:16])[CH2:13][CH2:12][NH:11][CH2:10]1)(=[O:7])[CH3:6].[CH3:17][C:18]1[CH:19]=[C:20]([CH:23]=[CH:24][CH:25]=1)[CH2:21]Cl.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>C(C(C)=O)C>[C:5]([NH:8][CH:9]1[CH2:10][N:11]([CH2:17][C:18]2[CH:25]=[CH:24][CH:23]=[C:20]([CH3:21])[CH:19]=2)[CH2:12][CH2:13][N:14]([CH3:16])[CH2:15]1)(=[O:7])[CH3:6]

参加物

7

反応物 5

HCID 175AcetateHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 12102m-Xylyl chlorideHCID 152061556-acetylamino-1-methylhexahydro-1H-1,4-diazepine

生成物 1

HCID 149989916-acetylamino-1-(3-methylbenzyl)-4-methylhexahydro-1H-1,4-diazepine

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of acetate of 6-acetylamino-1-methylhexahydro-1H-1,4-diazepine (3.0 g), 3-methylbenzyl chloride (3.5 g), potassium carbonate (17 g), sodium iodide (0.1 g) and methyl ethyl ketone (200 ml) is refluxed with stirring for 16 hours. The reaction mixture is filtered, and the filtrate is concentrated under reduced pressure. The residue is chromatographed on silica gel with elution of chloroform-methanol (20:1). Fractions containing the title compound are pooled and evaporated under reduced pressure to give the title compound as an oil.

後処理

  1. temperatureis refluxed
  2. filtrationThe reaction mixture is filtered
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. customThe residue is chromatographed on silica gel with elution of chloroform-methanol (20:1)
  5. additionFractions containing the title compound
  6. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-ad9e5766f2a34d56ae5126485c82708d
出典データセット
uspto-grants-1992_11
特許番号
US05166341

関連ノート

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