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

HRID 1081318
ノート
印刷プレビュー

反応式

HRID 1081318 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].[BH4-].[Na+]>CO>[F:39][C:3]([F:2])([F:40])[C:4]1[CH:5]=[C:6]([CH:32]=[C:33]([C:35]([F:37])([F:36])[F:38])[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])[CH2:16][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

4

反応物 2

HCID 4311764Sodium borohydrideHCID 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 23364122N-[3,5-bis(trifluoromethyl)benzyl]-5-(4-fluorophenyl)-1,2,7,8-tetrahydro-N,1,7-trimethyl-8-oxo-6-pyrido[3,4-b]pyridinecarboxamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of the compound (310 mg) obtained in Example 29 in methanol (15 ml) was added portionwise sodium borohydride (50 mg) at room temperature while stirring. This mixture was stirred for 15 minutes at room temperature, which was then concentrated. To the concentrate was added ethyl acetate, which was washed with water and dried, then the solvent was distilled off to leave N-[3,5-bis(trifluoromethyl)benzyl]-5-(4-fluorophenyl)-1,2,7,8-tetrahydro-N,1,7-trimethyl-8-oxo-6-pyrido[3,4-b]pyridinecarboxamide as a pale yellow oily product [NMR (200 MHz,CDCl3) ppm: 2.70(3H,s), 3.16(3H,s), 3.49(3H,s), 3.49(1H,m), 3.88(1H,m), 4.29(1H,d,J=14.6 Hz), 4.66(1H,d,J=14.6 Hz), 5.62(1H,m), 5.77(1H,d,J=13 Hz), 6.84-7.26(4H,m), 7.53(2H,s), 7.81(1H,s)].

後処理

  1. stirringThis mixture was stirred for 15 minutes at room temperature
  2. concentrationwhich was then concentrated
  3. additionTo the concentrate was added ethyl acetate, which
  4. washwas washed with water
  5. customdried
  6. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-619cad36a96f49e8938866dbf7324d27
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