Water → 4-[[2-Methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]nitrobenzene

HRID 427278ノート

反応式

HRID 427278 の反応式
[C:1]([NH2:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].O=[C:12]([CH3:24])[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=1.N1CCCCC1.O>C1C=CC=CC=1>[CH3:24][C:12]1([CH2:13][O:14][C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=2)[NH:10][C:1](=[O:9])[C:2]2[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=2[O:4]1

参加物

6

反応物 4

HCID 962Water2 回HCID 5147SalicylamideHCID 8082PiperidineHCID 3085071-(4-Nitrophenoxy)propan-2-one

生成物 1

HCID 183569464-[[2-Methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]nitrobenzene収率 86%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a stirred mixture of salicylamide (6.85 g, 50 mmol) and 4-[2-oxo-propoxy]nitrobenzene (9.75 g, 50 mmol) in benzene (500 mL) was added piperidine (0.52 mL, 5 mmol). The reaction mixture was immersed in a pre-heated oil bath (˜100° C.) and refluxed for 10 h with continuous removal of water using Dean-Stark water separator. The reaction mixture was cooled to room temperature End the precipitated brown coloured solid was filtered, washed with benzene and dried to afford the title compound (13.5 g, 86%).

後処理

  1. customThe reaction mixture was immersed in a pre-heated oil bath
  2. filtrationwas filtered
  3. washwashed with benzene
  4. customdried

出典と根拠

ORDレコード
ord-3d08c324cdf244e9b7acf322362868dc
出典データセット
uspto-grants-2001_11
特許番号
US06313113B1

反応ノート

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