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

HRID 1294480노트

반응식

HRID 1294480 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 sub-title 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-cdf94016d21d4f8bbccb56f6417e469e
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07241757B2

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