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Boron trifluoride → HCID 136389335、化合物

HRID 2422573
ノート
印刷プレビュー

反応式

HRID 2422573 の反応式
C[O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:18]([CH3:19])[C:17](=[O:20])[C:16]3[C:11](=[C:12]([CH3:21])[CH:13]=[CH:14][CH:15]=3)[N:10]=2)=[CH:5][CH:4]=1.B(F)(F)F.[OH-].[Na+]>ClCCl.C(OCC)(=O)C>[OH:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[N:18]([CH3:19])[C:17](=[O:20])[C:16]3[C:11](=[C:12]([CH3:21])[CH:13]=[CH:14][CH:15]=3)[N:10]=2)=[CH:7][CH:8]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6356Boron trifluorideHCID 14798Sodium HydroxideHCID 672445924(3H)-Quinazolinone, 2-(4-methoxyphenyl)-3,8-dimethyl-

生成物 1

HCID 136389335HCID 136389335、化合物収率 80.3%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate
溶媒

反応条件

温度
-78 °C

実験手順

2-(4-Methoxyphenyl)-3,8-dimethyl-4(3H)-quinazolinone (2.02 g, 7.20 mmol) was dissolved in dichloromethane (10 ml), stirred at −78° C., then boron trifluoride (1.0 M in CH2 Cl2, 21.6 ml) was added thereto, gradually heated up to room temperature, and stirred at that temperature for 12 hours. The reaction solution was diluted with ethyl acetate, and with cooling with ice, this was poured into aqueous 1 N sodium hydroxide solution, and extracted with ethyl acetate. The organic layer was washed with 1 N hydrochloric acid and saturated saline water, and dried with magnesium sulfate. The organic layer was concentrated under reduced pressure to obtain the intended compound (1.54 g, 80%) as a pale yellow solid.

後処理

  1. temperaturegradually heated up to room temperature
  2. stirringstirred at that temperature for 12 hours
  3. temperaturewith cooling with ice
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with 1 N hydrochloric acid and saturated saline water
  6. dry with materialdried with magnesium sulfate
  7. concentrationThe organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-9ee45a0b7a5840cf85aa0ff80a6626d5
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07960394B2

反応ノート

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