Calcium hypochlorite → 6-Chloro-8-difluoromethoxychroman-4-one

HRID 353248노트

반응식

HRID 353248 반응식
[Cl:1][O-].[Ca+2].Cl[O-].[F:6][CH:7]([F:20])[O:8][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:18]=1[O:17][CH2:16][CH2:15][C:14]2=[O:19]>O.C(O)(=O)C.C(#N)C.O>[Cl:1][C:11]1[CH:12]=[C:13]2[C:18](=[C:9]([O:8][CH:7]([F:6])[F:20])[CH:10]=1)[O:17][CH2:16][CH2:15][C:14]2=[O:19]

참가 물질

6

반응물 2

HCID 24504Calcium hypochloriteHCID 227083468-Difluoromethoxychroman-4-one

생성물 1

HCID 227083496-Chloro-8-difluoromethoxychroman-4-one수율 93%

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 21899381Acetic acid--water (1/1)용매

실험 절차

To a solution of calcium hypochlorite (29.4 g, 137.8 mmol) in water:acetic acid (125:9.5) was added a solution of 8-difluoromethoxychroman-4-one (7.4 g, 34.6 mmol, see step (iv) above) in acetonitrile (20 mL), whereafter the reaction mixture was stirred overnight. The mixture was diluted with water and extracted with ether (3×) and with EtOAc (1×). The combined organic layers were washed with water (3×), dried (Na2SO4) and evaporated, yielding 8.0 g (93%) of the subtitle compound.

후처리

  1. extractionextracted with ether (3×) and with EtOAc (1×)
  2. washThe combined organic layers were washed with water (3×)
  3. dry with materialdried (Na2SO4)
  4. customevaporated

출처 및 근거

ORD 기록
ord-8efa8896b30c49c487ad764f0aac41cd
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06750243B1

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