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Boron Trichloride → (3R)-3-ethyl-7-fluoro-4-(4-hydroxybenzoyl)-1-methyl-3,4-dihydroquinoxalin-2(1H)-one

HRID 898215
ノート
印刷プレビュー

反応式

HRID 898215 の反応式
[CH2:1]([C@H:3]1[N:12]([C:13](=[O:22])[C:14]2[CH:19]=[CH:18][C:17]([O:20]C)=[CH:16][CH:15]=2)[C:11]2[C:6](=[CH:7][C:8]([F:23])=[CH:9][CH:10]=2)[N:5]([CH3:24])[C:4]1=[O:25])[CH3:2].B(Cl)(Cl)Cl>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C(Cl)Cl>[CH2:1]([C@H:3]1[N:12]([C:13](=[O:22])[C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=2)[C:11]2[C:6](=[CH:7][C:8]([F:23])=[CH:9][CH:10]=2)[N:5]([CH3:24])[C:4]1=[O:25])[CH3:2]
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

5

反応物 2

HCID 25135Boron TrichlorideHCID 69223654(3R)-3-ethyl-7-fluoro-4-(4-methoxybenzoyl)-1-methyl-3,4-dihydroquinoxalin-2(1H)-one

生成物 1

HCID 11709655(3R)-3-ethyl-7-fluoro-4-(4-hydroxybenzoyl)-1-methyl-3,4-dihydroquinoxalin-2(1H)-one収率 88.6%

試薬・触媒・溶媒 2

HCID 67553Tetrabutylammonium Iodide触媒HCID 6344Dichloromethane
溶媒
2 回

反応条件

温度
0 °C

実験手順

To a stirred solution of (3R)-3-ethyl-7-fluoro-4-(4-methoxybenzoyl)-1-methyl-3,4 dihydroquinoxalin-2(1H)-one (0.19 g, 0.55 mmol) and tetrabutylammonium iodide (0.41 g, 1.1 mmol) in methylene chloride (5 mL), under nitrogen, at −78° C., was added a 1.0 M solution of boron trichloride in methylene chloride (2.8 mL, 2.8 mmol). Stirring was continued at −78° C. for 5 minutes, and the reaction was warmed to 0° C. where it was stirred for 5 h. The reaction was quenched by the addition of ice water, and the resulting mixture was stirred for 10 min. The layers were separated. The organic layer was washed with water and brine and dried over magnesium sulfate. Evaporation of the solvent and purification by eluting it through a short plug of silica gel with 75% hexane/EtOAc gave 0.16 g (88%) of (3R)-3-ethyl-7-fluoro-4-(4-hydroxybenzoyl)-1-methyl-3,4-dihydroquinoxalin-2(1H)-one. [α]D25=−300° (c=0.009 G/ML, DMSO); MS (ESI) m/z 329 ([M+H]+); MS (ESI) m/z 327 ([M−H]−); HRMS: calcd for C18H17FN2O3, 328.1223; found (ESI+), 329.13036; Anal. Calcd for C18H17FN2O3: C, 65.85; H, 5.22; N, 8.53. Found: C, 65.73; H, 5.46; N, 8.28.

後処理

  1. stirringwas stirred for 5 h
  2. customThe reaction was quenched by the addition of ice water
  3. stirringthe resulting mixture was stirred for 10 min
  4. customThe layers were separated
  5. washThe organic layer was washed with water and brine
  6. dry with materialdried over magnesium sulfate
  7. customEvaporation of the solvent and purification
  8. washby eluting it through a short plug of silica gel with 75% hexane/EtOAc

出典と根拠

ORDレコード
ord-823f9168a24346eb86dfbb95ef91d0f9
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07351709B2

反応ノート

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