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Boron trifluoride → HCID 136389335, 화합물

HRID 2422573
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HRID 2422573 반응식
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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 136389335HCID 136389335, 화합물수율 80.3%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate
용매

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온도
-78 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9ee45a0b7a5840cf85aa0ff80a6626d5
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07960394B2

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