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

HRID 9348

반응식

HRID 9348 반응식
[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

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178418737HCID 178418737, 화합물

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-124d1086d4d44e1a9c954932a0b1a5e1
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091214B2

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