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Benzyl Bromide → 4-Benzyloxy-6-fluoro-naphthalene-2-carboxylic acid methyl ester

HRID 2363807
ノート
印刷プレビュー

反応式

HRID 2363807 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:14]=[C:13]([OH:15])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([F:16])[CH:11]=2)[CH:6]=1)=[O:4].C([O-])([O-])=O.[K+].[K+].[CH2:23](Br)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(OCC)(=O)C>CN(C=O)C.[N+](CCCC)(CCCC)(CCCC)CCCC.[I-].O>[CH3:1][O:2][C:3]([C:5]1[CH:14]=[C:13]([O:15][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([F:16])[CH:11]=2)[CH:6]=1)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 7498Benzyl BromideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 59326505Methyl 6-fluoro-4-hydroxy-2-naphthoate

生成物 1

HCID 593265854-Benzyloxy-6-fluoro-naphthalene-2-carboxylic acid methyl ester収率 88.2%

試薬・触媒・溶媒 3

HCID 67553
Tetrabutylammonium Iodide
触媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 6-fluoro-4-hydroxy-naphthalene-2-carboxylic acid methyl ester (3.7 g, 16.8 mmol) in dry DMF (40 mL) was added K2CO3 (3.25 g, 23.5 mmol), benzyl bromide (3.44 g, 20.2 mmol) and Bu4NI (0.02 g) simultaneously at room temperature under nitrogen. The reaction mixture was stirred for 3 hours at room temperature. The mixture was diluted with water (60 mL) and extracted with ethyl acetate (2×100 mL). The combined organic extracts were washed with water (30 mL), brine (30 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to obtain the crude product. Silica gel column chromatography (2%-5% ethyl acetate in hexanes) afforded 4-benzyloxy-6-fluoro-naphthalene-2-carboxylic acid methyl ester (4.6 g, 88%) as an off-white solid. MS cald. for C19H16FO3 [(M+H)+]: 311, obsd. 311.0.

後処理

  1. extractionextracted with ethyl acetate (2×100 mL)
  2. washThe combined organic extracts were washed with water (30 mL), brine (30 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customto obtain the crude product

出典と根拠

ORDレコード
ord-7b21e1f395954eefab4b3249891b037f
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08691993B2

反応ノート

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