Ethanol, reaction products with ammonia, distn. residues → 2-(6,7-Dihydro-8H-indeno[5,4-d][1,3]oxazol-8-ylidene)ethanamine

HRID 883201ノート

反応式

HRID 883201 の反応式
[O:1]1[C:5]2[C:6]3[C:7](=[CH:13][C:14]#[N:15])[CH2:8][CH2:9][C:10]=3[CH:11]=[CH:12][C:4]=2[N:3]=[CH:2]1.N.C(O)C>C(O)C.[Co]>[O:1]1[C:5]2[C:6]3[C:7](=[CH:13][CH2:14][NH2:15])[CH2:8][CH2:9][C:10]=3[CH:11]=[CH:12][C:4]=2[N:3]=[CH:2]1

参加物

5

反応物 2

HCID 22020343Ethanol, reaction products with ammonia, distn. residuesHCID 67353458(6,7-Dihydro-8H-indeno[5,4-d][1,3]oxazol-8-ylidene)acetonitrile

生成物 1

HCID 673539192-(6,7-Dihydro-8H-indeno[5,4-d][1,3]oxazol-8-ylidene)ethanamine収率 28.1%

試薬・触媒・溶媒 2

HCID 104730Cobalt触媒HCID 702Ethanol溶媒

実験手順

To a solution of (6,7-dihydro-8H-indeno[5,4-d][1,3]oxazol-8-ylidene)acetonitrile (210 mg, 1.07 mmol) in ethanol (8 mL) were added Raney cobalt (2 g) and 2N ammonia/ethanol solution (4 mL), and the mixture was stirred at room temperature for 5 hr under a hydrogen atmosphere. The catalyst was filtered off using celite, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane=50/50→100/0) to give the title compound (60.2 mg, yield 28%).

後処理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane=50/50→100/0)

出典と根拠

ORDレコード
ord-baec5dadb4844966b8e71c7f3e3cba6f
出典データセット
uspto-grants-2012_08
特許番号
US08236837B2

反応ノート

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