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Sodium Hydroxide → N-[3,5-Bis(trifluoromethyl)benzyl]-5-(4-fluorophenyl)-1,2,7,8-tetrahydro-N,1,7-trimethyl-2,8-dioxo-6-pyrido [3,4-b]pyridinecarboxamide

HRID 1081320
ノート
印刷プレビュー

反応式

HRID 1081320 の反応式
[I-].[F:2][C:3]([F:40])([F:39])[C:4]1[CH:5]=[C:6]([CH:32]=[C:33]([C:35]([F:38])([F:37])[F:36])[CH:34]=1)[CH2:7][N:8]([CH3:31])[C:9]([C:11]1[N:21]([CH3:22])[C:20](=[O:23])[C:14]2=[N+:15]([CH3:19])[CH:16]=[CH:17][CH:18]=[C:13]2[C:12]=1[C:24]1[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=1)=[O:10].[OH-:41].[Na+]>[Fe-3](C#N)(C#N)(C#N)(C#N)(C#N)C#N.[K+].[K+].[K+].C1COCC1>[F:40][C:3]([F:2])([F:39])[C:4]1[CH:5]=[C:6]([CH:32]=[C:33]([C:35]([F:37])([F:38])[F:36])[CH:34]=1)[CH2:7][N:8]([CH3:31])[C:9]([C:11]1[N:21]([CH3:22])[C:20](=[O:23])[C:14]2[N:15]([CH3:19])[C:16](=[O:41])[CH:17]=[CH:18][C:13]=2[C:12]=1[C:24]1[CH:25]=[CH:26][C:27]([F:30])=[CH:28][CH:29]=1)=[O:10]
参加物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 14798Sodium HydroxideHCID 233640506-[N-[3,5-Bis(trifluoromethyl)benzyl]-N-methylamino carbonyl]-5-(4-fluorophenyl)-7,8-dihydro-1,7-dimethyl-8-oxopyrido[3,4-b]pyridinium iodide

生成物 1

HCID 22355428N-[3,5-Bis(trifluoromethyl)benzyl]-5-(4-fluorophenyl)-1,2,7,8-tetrahydro-N,1,7-trimethyl-2,8-dioxo-6-pyrido [3,4-b]pyridinecarboxamide

試薬・触媒・溶媒 2

HCID 178511488HCID 178511488、化合物触媒
HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 6-[N-[3,5-bis(trifluoromethyl)benzyl]-N-methylaminocarbonyl]-5-(4-fluorophenyl)-7,8-dihydro-1,7-dimethyl-8-oxopyrido[3,4-b]pyridinium iodide (Example 29) (100 mg), THF (3 ml), potassium ferricyanide (500 mg) and 1N-NaOH was stirred for 15 hours. The solvent was distilled off. To the residue was added ethyl acetate, and the mixture was washed with water and dried, then the solvent was distilled off. The residue was subjected to a silica-gel column chromatography (ethyl acetate) for separation and purification to afford the above-titled compound as colorless crystals (35 mg), m.p.210°-212° C. (recrystallized from ethyl acetate-isopropyl ether).

後処理

  1. distillationThe solvent was distilled off
  2. additionTo the residue was added ethyl acetate
  3. washthe mixture was washed with water
  4. customdried
  5. distillationthe solvent was distilled off
  6. customThe residue was subjected to a silica-gel column chromatography (ethyl acetate) for separation and purification
  7. customto afford
  8. customthe above-titled compound as colorless crystals (35 mg), m.p.210°-212° C. (recrystallized from ethyl acetate-isopropyl ether)

出典と根拠

ORDレコード
ord-dd00fcd111ea4338ba4de17e4e8d3172
出典データセット
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05585385

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート