Bromide ion → HCID 84689561、化合物

HRID 607190ノート

反応式

HRID 607190 の反応式
[CH:1]([C:4]1[NH:9][C:8](=O)[C:7]([C:11]#[N:12])=[CH:6][CH:5]=1)([CH3:3])[CH3:2].[Br-:13].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.O>C1(C)C=CC=CC=1>[Br:13][C:8]1[N:9]=[C:4]([CH:1]([CH3:3])[CH3:2])[CH:5]=[CH:6][C:7]=1[C:11]#[N:12]

参加物

6

反応物 4

HCID 259Bromide ionHCID 962WaterHCID 14812Phosphorus oxide (P4O10)HCID 105831136-Isopropyl-2-oxo-1,2-dihydropyridine-3-carbonitrile

生成物 1

HCID 84689561HCID 84689561、化合物収率 93.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

To a solution of the product of Example 36B (4.35 g, 0.0269 mol), tertrabutylammonium bromide (10.4 g, 0.0323 mol) and phosphorous pentoxide (8.01 g, 1.05 mol) in toluene (80 mL) was heated under reflux for 5 hours. The reaction mixture was then cooled to room temperature, water (80 mL) was added, and the mixture was stirred for 2 h at room temperature. The reaction mixture was diluted with toluene (20 mL) and the organic layer separated. The aqueous layer was washed with toluene (50 mL) and the combined organic layers were washed with brine (50 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum to provide the title product as a yellow oil (5.64 g, 93%).

後処理

  1. temperatureunder reflux for 5 hours
  2. customthe organic layer separated
  3. washThe aqueous layer was washed with toluene (50 mL)
  4. washthe combined organic layers were washed with brine (50 mL)
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-38b42360040545d0ac00baa809f88076
出典データセット
uspto-grants-2011_03
特許番号
US07915411B2

反応ノート

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