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Sodium hydride → 2-[4-[N-(tert-butoxycarbonyl)-N-methylamino]-3-fluorophenyl]-6,8-difluoro-5-(4-pentenylamino)-4H-benzopyran-4-one

HRID 1736148
ノート
印刷プレビュー

反応式

HRID 1736148 の反応式
[NH2:1][C:2]1[C:7]2[C:8](=[O:28])[CH:9]=[C:10]([C:12]3[CH:17]=[CH:16][C:15]([N:18]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH3:19])=[C:14]([F:27])[CH:13]=3)[O:11][C:6]=2[C:5]([F:29])=[CH:4][C:3]=1[F:30].[H-].[Na+].Br[CH2:34][CH2:35][CH2:36][CH:37]=[CH2:38].[Cl-].[NH4+]>CN(C)C=O>[C:23]([O:22][C:20]([N:18]([C:15]1[CH:16]=[CH:17][C:12]([C:10]2[O:11][C:6]3[C:5]([F:29])=[CH:4][C:3]([F:30])=[C:2]([NH:1][CH2:38][CH2:37][CH2:36][CH:35]=[CH2:34])[C:7]=3[C:8](=[O:28])[CH:9]=2)=[CH:13][C:14]=1[F:27])[CH3:19])=[O:21])([CH3:24])([CH3:25])[CH3:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 24758Sodium hydride2 回HCID 25517Ammonium ChlorideHCID 707041-Pentene, 5-bromo-2 回HCID 19434922HCID 19434922、化合物

生成物 1

HCID 194347972-[4-[N-(tert-butoxycarbonyl)-N-methylamino]-3-fluorophenyl]-6,8-difluoro-5-(4-pentenylamino)-4H-benzopyran-4-one収率 24%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

852 mg (2.03mmol) of the resulting 5-amino-2-[4-[N-(tert-butoxycarbonyl)-N-methylamino]-3-fluorophenyl]-6,8-difluoro-4H-1-benzopyran-4-one was dissolved in 30 ml of dimethylformamide under argon atmosphere, 165 mg of sodium hydride (60% oil dispersion) and 0.48 ml of 5-bromo-1-pentene were added under ice-cooling and the mixture was stirred at room temperature for 2 hours. 85 mg of sodium hydride (60% oil dispersion) and 0.24 ml of 5-bromo-1-pentene were added and the mixture was stirred for additional 1 hour. An aqueous saturated solution of ammonium chloride was added to the reaction solution and the mixture was extracted twice with ethyl acetate. The organic layer was washed with an aqueous saturated solution of sodium chloride and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=7:1) to give 239 mg (24%) of 2-[4-[N-(tert-butoxycarbonyl)-N-methylamino]-3-fluorophenyl]-6,8-difluoro-5-(4-pentenylamino)-4H-benzopyran-4-one.

後処理

  1. temperaturecooling
  2. stirringthe mixture was stirred for additional 1 hour
  3. extractionthe mixture was extracted twice with ethyl acetate
  4. washThe organic layer was washed with an aqueous saturated solution of sodium chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=7:1)

出典と根拠

ORDレコード
ord-e3f798de462342c78cbfb06c2ad07d35
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05539112

反応ノート

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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