Water → HCID 57555222、化合物

HRID 220816ノート

反応式

HRID 220816 の反応式
C(=O)([O-])[O-].[K+].[K+].I[CH3:8].[CH:9]1([NH:15][C:16]2[C:17]([NH2:22])=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.O>CN(C=O)C>[CH:9]1([NH:15][C:16]2[C:17]([NH:22][CH3:8])=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 1517328N-(2-aminophenyl)-N-cyclohexylamine

生成物 1

HCID 57555222HCID 57555222、化合物収率 39%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Potassium carbonate (2.45 g, 17.7 mmol) and iodomethane (0.81 ml, 13.0 mmol) were added to a solution of N-cyclohexyl-benzene-1,2-diamine from Example E26.2 (2.25 g, 11.8 mmol) in DMF (10 ml). The mixture was stirred for 6 h at room temperature then poured into water and extracted with EtOAc. The organic layer was washed with water then brine, dried and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (eluant; 5% EtOAc:95% hexane) to yield the title compound (950 mg, 39%).

後処理

  1. extractionextracted with EtOAc
  2. washThe organic layer was washed with water
  3. dry with materialbrine, dried
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography on silica gel (eluant; 5% EtOAc:95% hexane)

出典と根拠

ORDレコード
ord-c29c950c60ad4e6287372633c148642e
出典データセット
uspto-grants-2012_06
特許番号
US08202858B2

反応ノート

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