Oxirane, [(2,3-dimethylphenoxy)methyl]- → HCID 13506762、化合物

HRID 1583440ノート

反応式

HRID 1583440 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:14]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[CH3:21])[C:13]2[C:12](=[O:22])[CH2:11][NH:10][CH2:9][C:8]=2[NH:7][C:6]=1[CH3:23])=[O:4].[CH3:24][C:25]1[C:35]([CH3:36])=[CH:34][CH:33]=[CH:32][C:26]=1[O:27][CH2:28][CH:29]1[O:31][CH2:30]1>CO>[CH3:1][O:2][C:3]([C:5]1[CH:14]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[CH3:21])[C:13]2[C:12](=[O:22])[CH2:11][N:10]([CH2:30][CH:29]([OH:31])[CH2:28][O:27][C:26]3[CH:32]=[CH:33][CH:34]=[C:35]([CH3:36])[C:25]=3[CH3:24])[CH2:9][C:8]=2[NH:7][C:6]=1[CH3:23])=[O:4]

参加物

4

反応物 2

HCID 12619677Oxirane, [(2,3-dimethylphenoxy)methyl]-HCID 12818458HCID 12818458、化合物

生成物 1

HCID 13506762HCID 13506762、化合物収率 41.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1,4,5,6,7,8-Hexahydro-2-methyl-4-(2-methylphenyl)-5-oxo-1,7-naphthyridine-3-carboxylic acid methyl ester (14.5 g), 6.8 g of 3-(2,3-dimethylphenoxy)-1,2-epoxypropane and 250 ml of methanol were combined and refluxed for 18 hours. The solvent was removed in vacuo. The residue was dissolved in diethyl ether and saturated with hydrogen chloride. The solid was separated and dried in vacuo at 75° C. for 18 hours. The solid was recrystallized from acetonitrile to obtain 7.7 g of the title compound as the hydrochloride salt, m.p. 220° C. dec.

後処理

  1. temperaturerefluxed for 18 hours
  2. customThe solvent was removed in vacuo
  3. dissolutionThe residue was dissolved in diethyl ether and saturated with hydrogen chloride
  4. customThe solid was separated
  5. customdried in vacuo at 75° C. for 18 hours
  6. customThe solid was recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-220563bc64f346139d61676428fe3e7a
出典データセット
uspto-grants-1985_11
特許番号
US04551534

反応ノート

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