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Boron tribromide → HCID 10976036, 화합물

HRID 504002
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HRID 504002 반응식
B(Br)(Br)Br.C[O:6][C:7]1[CH:16]=[CH:15][C:14]([CH3:17])=[C:13]2[C:8]=1[CH2:9][CH2:10][C:11](=[O:18])[NH:12]2>ClCCl>[OH:6][C:7]1[CH:16]=[CH:15][C:14]([CH3:17])=[C:13]2[C:8]=1[CH2:9][CH2:10][C:11](=[O:18])[NH:12]2
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참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 66597026HCID 66597026, 화합물

생성물 1

HCID 10976036HCID 10976036, 화합물수율 101.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A 2N dichloromethane solution (52 ml) of boron tribromide was added dropwise at −20° C. to a dichloromethane solution (100 ml) of 5-methoxy-8-methyl-3,4-dihydro-1H-quinolin-2-one (10.0 g). After stirring for 1 hour, the reaction mixture was poured into ice water and separated into layers. The organic layer was washed twice with water, washed with a saturated sodium chloride solution, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was recrystallized from an ethyl acetate-diethyl ether mixed solvent to thereby obtain 9.4 g (yield: quantitative) of 5-hydroxy-8-methyl-3,4-dihydro-1H-quinolin-2-one as a white powder.

후처리

  1. customseparated into layers
  2. washThe organic layer was washed twice with water
  3. washwashed with a saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from an ethyl acetate-diethyl ether mixed solvent

출처 및 근거

ORD 기록
ord-0f90844cf5a4483eb02818e12ef538d9
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07777038B2

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