Ethanol, reaction products with ammonia, distn. residues → HCID 54094556、化合物

HRID 1977985ノート

反応式

HRID 1977985 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][CH2:9][C:10]2=[CH:13][C:14]#[N:15])=[CH:5][CH:4]=1.N.C(O)C>C(O)C.[Ni]>[NH2:15][CH2:14][CH:13]=[C:10]1[C:11]2[C:6](=[CH:5][CH:4]=[C:3]([O:2][CH3:1])[CH:12]=2)[CH2:7][CH2:8][CH2:9]1

参加物

5

反応物 2

HCID 22020343Ethanol, reaction products with ammonia, distn. residuesHCID 54328648(E)-2-(7-methoxy-3,4-dihydronaphthalen-1(2H)-ylidene)acetonitrile

生成物 1

HCID 54094556HCID 54094556、化合物収率 80%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

To a solution of (1,2,3,4-tetrahydro-7-methoxy-1-naphthylidene)acetonitrile (15.0 g, 25 mmol) in ethanol (100 ml) were added a saturated ammonia/ethanol solution (30 ml) and Raney nickel (W-2, 3 g). The reaction mixture was stirred for 8 hours at 50° C. under hydrogen atmosphere (3-4 kgf /cm2). The Raney nickel was filtered off, then the solvent was distilled off under reduced pressure to give the above-titled compound (a mixture of isomers (20.4 g, yield 80%, oil). This compound was used in the subsequent reaction without further purification.

後処理

  1. filtrationThe Raney nickel was filtered off
  2. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-9ed2a8b2b3be43028dc7b94878229e42
出典データセット
uspto-grants-2001_05
特許番号
US06235789B1

反応ノート

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