Ethanol → N-Cycloheptyl-[(2-fluorenyl)methyl]amine

HRID 256622

反応式

HRID 256622 の反応式
[CH:1]([C:3]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:6][C:5]=2[CH:4]=1)=O.[CH:16]1([NH2:23])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.C(O)C.[BH4-].[Na+]>O>[CH:16]1([NH:23][CH2:1][C:3]2[CH:15]=[CH:14][C:13]3[C:12]4[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=4)[CH2:6][C:5]=3[CH:4]=2)[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1

参加物

6

反応物 4

HCID 702EthanolHCID 2899CycloheptylamineHCID 34804Fluorene-2-carboxaldehydeHCID 4311764Sodium borohydride

生成物 1

HCID 15284282N-Cycloheptyl-[(2-fluorenyl)methyl]amine収率 92.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-Formylfluorene (2.27 g, 11.7 mmol) and cycloheptylamine (1.39 g, 12.3 mmol) were heated together at 120° C. for 14 hrs. After cooling, the reaction mixture was distilled under reduced pressure. Then, ethanol (30 ml) and sodium borohydride (0.44 g, 11.7 mmol) were added to the residue and the mixture was stirred for 0.5 hr. The mixture was then diluted with water (100 ml) and extracted with chloroform (80 ml×2 times). The organic layer was dried over anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure to give 3.15 g of a pale yellow solid residue.

後処理

  1. temperatureAfter cooling
  2. distillationthe reaction mixture was distilled under reduced pressure
  3. extractionextracted with chloroform (80 ml×2 times)
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. distillationThe solvent was then distilled off under reduced pressure

出典と根拠

ORDレコード
ord-a8a992336120472ea7f27f226b1f77c7
出典データセット
uspto-grants-1993_11
特許番号
US05258405

関連ノート

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