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Boron tribromide → HCID 10976036、化合物

HRID 504002
ノート
印刷プレビュー

反応式

HRID 504002 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 66597026HCID 66597026、化合物

生成物 1

HCID 10976036HCID 10976036、化合物収率 101.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0f90844cf5a4483eb02818e12ef538d9
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07777038B2

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