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Nitric Acid → 2-Tert-butyl-4-fluoro-5-nitrophenyl methyl carbonate

HRID 470015
ノート
印刷プレビュー

反応式

HRID 470015 の反応式
[C:1](=[O:16])([O:14][CH3:15])[O:2][C:3]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:4]=1[C:10]([CH3:13])([CH3:12])[CH3:11].[N+:17]([O-:20])([OH:19])=[O:18]>OS(O)(=O)=O>[C:1](=[O:16])([O:14][CH3:15])[O:2][C:3]1[CH:8]=[C:7]([N+:17]([O-:19])=[O:18])[C:6]([F:9])=[CH:5][C:4]=1[C:10]([CH3:11])([CH3:12])[CH3:13].[C:1](=[O:16])([O:14][CH3:15])[O:2][C:3]1[C:8]([N+:17]([O-:20])=[O:18])=[CH:7][C:6]([F:9])=[CH:5][C:4]=1[C:10]([CH3:11])([CH3:12])[CH3:13]
参加物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 944Nitric AcidHCID 574702152-Tert-butyl-4-fluorophenyl methyl carbonate

生成物 2

HCID 574702162-Tert-butyl-4-fluoro-5-nitrophenyl methyl carbonate収率 55%HCID 574702172-Tert-butyl-4-fluoro-6-nitrophenyl methyl carbonate収率 12%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

To a solution of 2-tert-butyl-4-fluorophenyl methyl carbonate (1.81 g, 8 mmol) in H2SO4 (98%, 1 mL) was added slowly a cooled mixture of H2SO4 (1 mL) and HNO3 (1 mL) at 0° C. The mixture was stirred for 2 h while warming to room temperature, poured into ice and extracted with diethyl ether. The ether extract was washed with brine, dried over MgSO4 and concentrated. The residue was purified by column chromatography (0-10% EtOAc—Hexane) to give 2-tert-butyl-4-fluoro-5-nitrophenyl methyl carbonate (C-7-a) (1.2 g, 55%) and 2-tert-butyl-4-fluoro-6-nitrophenyl methyl carbonate (C-6-a) (270 mg, 12%). 2-tert-Butyl-4-fluoro-5-nitrophenyl methyl carbonate (C-7-a): 1H NMR (400 MHz, DMSO-d6) δ 8.24 (d, J=7.1 Hz, 1H), 7.55 (d, J=13.4 Hz, 1H), 3.90 (s, 3H), 1.32 (s, 9H). 2-tert-butyl-4-fluoro-6-nitrophenyl methyl carbonate (C-6-a): 1H NMR (400 MHz, DMSO-d6) δ 8.04 (dd, J=7.6, 3.1 Hz, 1H), 7.69 (dd, J=10.1, 3.1 Hz, 1H), 3.91 (s, 3H), 1.35 (s, 9H).

後処理

  1. additionpoured into ice
  2. extractionextracted with diethyl ether
  3. extractionThe ether extract
  4. washwas washed with brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography (0-10% EtOAc—Hexane)

出典と根拠

ORDレコード
ord-e400d020856d46f39fedcfd23eab31d6
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629162B2

反応ノート

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