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Tetrafluoroboric acid → HCID 69743175、化合物

HRID 1760046
ノート
印刷プレビュー

反応式

HRID 1760046 の反応式
F[B-](F)(F)F.[H+].N([O-])=O.[Na+].O1CCOCC1.N[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[NH:24][C@@H:25]([C:42]([CH3:45])([CH3:44])[CH3:43])[C:26]([N:28]1[CH2:37][CH2:36][C:35]2[C:30](=[CH:31][C:32]([O:40][CH3:41])=[C:33]([O:38][CH3:39])[CH:34]=2)[CH2:29]1)=[O:27]>[Cu-]=O.O>[C:19]1([NH:24][C@@H:25]([C:42]([CH3:45])([CH3:44])[CH3:43])[C:26]([N:28]2[CH2:37][CH2:36][C:35]3[C:30](=[CH:31][C:32]([O:40][CH3:41])=[C:33]([O:38][CH3:39])[CH:34]=3)[CH2:29]2)=[O:27])[CH:20]=[CH:21][CH:22]=[CH:23][CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 28118Tetrafluoroboric acidHCID 312751,4-Dioxane2 回HCID 20748464HCID 20748464、化合物HCID 23668193Sodium Nitrite

生成物 1

HCID 69743175HCID 69743175、化合物収率 71.1%

試薬・触媒・溶媒 2

HCID 178419072HCID 178419072、化合物
触媒
HCID 962Water溶媒

実験手順

Tetrafluoroboric acid (1.5 ml) and an aqueous sodium nitrite solution (20 mg/0.2 ml, 0.29 mmol) were added, at 0° C., to a dioxane (2 ml) solution of (2S)-2-[(2aminophenyl)amino]-1-(6,7-dimethoxy-1,2,3,4-tetrahydroisoquinolin-2-yl)-3,3dimethylbutan-1-one (100 mg, 0.25 mmol) obtained in Example 25, and the mixture was stirred at that temperature for 30 minutes. Copper (I) oxide (75 mg, 0.52 mmol) was added to the reaction solution, and the mixture was stirred for 30 minutes. Dioxane (2 ml) and water (10 ml) were added to the mixture, and the mixture was concentrated under reduced pressure. The residue was extracted twice with chloroform (each 5 ml), and the extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel thin layer chromatography using hexane and ethyl acetate (2:1) as an eluent to obtain the captioned compound (68.0 mg, 70%) as a green oily substance.

後処理

  1. stirringthe mixture was stirred for 30 minutes
  2. concentrationthe mixture was concentrated under reduced pressure
  3. extractionThe residue was extracted twice with chloroform (each 5 ml), and the extract
  4. dry with materialwas dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel thin layer chromatography

出典と根拠

ORDレコード
ord-4445743d773743b89cf88c177901d8de
出典データセット
uspto-grants-2005_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06838465B2

反応ノート

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