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Dimethylformamide → 2-Bromo-3-fluoro-6-nitrobenzamide

HRID 471605
ノート
印刷プレビュー

反応式

HRID 471605 の反応式
[Br:1][C:2]1[C:10]([F:11])=[CH:9][CH:8]=[C:7]([N+:12]([O-:14])=[O:13])[C:3]=1[C:4](O)=[O:5].C[N:16](C=O)C.C(Cl)(=O)C(Cl)=O>C1COCC1>[Br:1][C:2]1[C:10]([F:11])=[CH:9][CH:8]=[C:7]([N+:12]([O-:14])=[O:13])[C:3]=1[C:4]([NH2:16])=[O:5]
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 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 598491772-Bromo-3-fluoro-6-nitrobenzoic acid

生成物 1

HCID 674009152-Bromo-3-fluoro-6-nitrobenzamide収率 42%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

2-Bromo-3-fluoro-6-nitrobenzoic acid (Example 134f) (24.83 g, 94.0) mmol, (mixture of two regioisomers) was dissolved in anhydrous THF (200 mL) under a nitrogen atmosphere at room temperature. Anhydrous DMF (0.75 mL) was added and the obtained mixture was cooled to 0° C. Oxalyl chloride (12.3 mL, 141 mmol) was slowly added and the reaction mixture was stirred at 0° C. for 10 min, and at room temperature for a further 2 h. The reaction was evaporated to dryness, suspended in anhydrous THF (100 mL) and added slowly to concentrated ammonium hydroxide (350 mL) at 0° C. After stirring for 45 minutes at 0° C. the mixture was extracted with CH2Cl2 (5×100 mL), and the organic extractions were then discarded. At this point the desired regioisomer existed as an insoluble precipitate in the aqueous layer, which was collected by filtration to give 10.3 g (42%) of 2-bromo-3-fluoro-6-nitrobenzamide which was used without further purification. 1H NMR (400 MHz, DMSO-d6) δ 8.27 (dd, J=8.8, 4.4 Hz, 1H), 8.10 (broad s, 1H), 7.95 (broad s, 1H), 7.66 (dd, J=9.6, 7.6 Hz, 1H).

後処理

  1. waitat room temperature for a further 2 h
  2. customThe reaction was evaporated to dryness
  3. additionadded slowly to concentrated ammonium hydroxide (350 mL) at 0° C
  4. stirringAfter stirring for 45 minutes at 0° C. the mixture
  5. extractionwas extracted with CH2Cl2 (5×100 mL)
  6. extractionthe organic extractions
  7. filtrationwas collected by filtration

出典と根拠

ORDレコード
ord-24fd52e0f8a5440bb678baff30e7196b
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08633186B2

反応ノート

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