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(E)-(6-methoxyindan-1-ylidene)acetonitrile → (E)-1-(2-Aminoethylidene)-6-methoxyindan

HRID 582201
ノート
印刷プレビュー

反応式

HRID 582201 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8]/[C:9]/2=[CH:12]\[C:13]#[N:14])=[CH:5][CH:4]=1.N.CO>C(O)C.[Co]>[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8]/[C:9]/2=[CH:12]\[CH2:13][NH2:14])=[CH:5][CH:4]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 11830118(E)-(6-methoxyindan-1-ylidene)acetonitrileHCID 21705897Ammonia methanol

生成物 1

HCID 10987044(E)-1-(2-Aminoethylidene)-6-methoxyindan収率 86%

試薬・触媒・溶媒 2

HCID 104730Cobalt触媒HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

To a solution of (E)-(6-methoxyindan-1-ylidene)acetonitrile (1.60 g, 8.64 mmol.) in ethanol (80 ml) were added a 2M ammonia/methanol solution (40 ml) and Raney cobalt (1.6 g). The reaction mixture was stirred, under hydrogen atmosphere (4 kgf/cm2) for 32 hours at 40° C. and for further 8 hours at 70° C. The Raney cobalt was filtered off, and then the solvent was distilled off. The residue was purified by means of a silica gel column chromatography (chloroform:methanol=9:1 to chloroform:methanol:triethylamine=90:8:2) to afford the titled compound (1.40 g, yield 86%, oily).

後処理

  1. waitfor further 8 hours at 70° C
  2. filtrationThe Raney cobalt was filtered off
  3. distillationthe solvent was distilled off
  4. customThe residue was purified by means of a silica gel column chromatography (chloroform:methanol=9:1 to chloroform:methanol:triethylamine=90:8:2)

出典と根拠

ORDレコード
ord-f082034c6aad4a69bf1d1e2e999859cd
出典データセット
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05922771

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート