Phosphorus oxychloride → 7-Bromo-4-chloro-3-nitroquinoline

HRID 9348

反応式

HRID 9348 の反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](O)=[C:7]([N+:12]([O-:14])=[O:13])[CH:8]=[N:9]2)=[CH:4][CH:3]=1.O=P(Cl)(Cl)[Cl:18]>>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([Cl:18])=[C:7]([N+:12]([O-:14])=[O:13])[CH:8]=[N:9]2)=[CH:4][CH:3]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178418737HCID 178418737、化合物

生成物 1

HCID 219843617-Bromo-4-chloro-3-nitroquinoline

実験手順

7-Bromo-3-nitroquinolin-4-ol (42 g, 156 millimoles (mmol)) was suspended in POCl3 (130 mL) and brought to 102° C. under an atmosphere of N2. After 45 min, all of the solids had dissolved, so the reaction was cooled to room temperature (RT). The resulting solids were collected by filtration, washed with H2O, and then partitioned with CH2Cl2 (3 L) and 2M Na2CO3 (500 mL). The organic layer was separated, washed with H2O (1×), dried over Na2SO4, filtered, and concentrated to afford 33.7 g of 7-bromo-4-chloro-3-nitroquinoline as a beige solid.

後処理

  1. custombrought to 102° C. under an atmosphere of N2
  2. dissolutionall of the solids had dissolved, so the reaction
  3. filtrationThe resulting solids were collected by filtration
  4. washwashed with H2O
  5. custompartitioned with CH2Cl2 (3 L) and 2M Na2CO3 (500 mL)
  6. customThe organic layer was separated
  7. washwashed with H2O (1×)
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-124d1086d4d44e1a9c954932a0b1a5e1
出典データセット
uspto-grants-2006_08
特許番号
US07091214B2

関連ノート

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