Ammonium Hydroxide → 6-phenoxy-2H-1-benzopyran-3-carboxaldehyde

HRID 466190노트

반응식

HRID 466190 반응식
[O:1]([C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][CH:14]=[CH:13][C:12]=2[CH:17]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:18](N1CCOCC1)=[O:19].P(Cl)(Cl)(Cl)=O.[OH-].[NH4+]>C(Cl)Cl>[O:1]([C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][C:14]([CH:18]=[O:19])=[CH:13][C:12]=2[CH:17]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 14923Ammonium HydroxideHCID 20417N-FormylmorpholineHCID 24813Phosphorus oxychlorideHCID 198156156-phenoxy-2H-1-benzopyran

생성물 1

HCID 149712656-phenoxy-2H-1-benzopyran-3-carboxaldehyde

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
60 °C

실험 절차

6-Phenoxy-2H-1-benzopyran (3.36 g, 15 mmol) and N-formylmorpholine (10.4 g, 90 mmol) are dissolved in 10.5 ml of methylene chloride and treated with phosphorus oxychloride (13.8 g, 90 mmol) at 0° C. over 15 minutes. The mixture is then heated at 60° C. for 27 hours, cooled and poured slowly into an ice-water mixture. The mixture is then neutralized with aqueous ammonium hydroxide, and extracted twice with methylene chloride. The combined organic extracts are washed with water, dried (MgSO4), and evaporated to give crude 6-phenoxy-2H-1-benzopyran-3-carboxaldehyde, which is used without further purification.

후처리

  1. temperaturecooled
  2. extractionextracted twice with methylene chloride
  3. washThe combined organic extracts are washed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-d06081969dae465aaa28a5bee1c87b47
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155130

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