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

HRID 1294480ノート

反応式

HRID 1294480 の反応式
[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]

参加物

6

反応物 2

HCID 24504Calcium hypochloriteHCID 227083468-Difluoromethoxychroman-4-one

生成物 1

HCID 227083496-Chloro-8-difluoromethoxychroman-4-one収率 93%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6342Acetonitrile溶媒HCID 21899381Acetic acid--water (1/1)溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cdf94016d21d4f8bbccb56f6417e469e
出典データセット
uspto-grants-2007_07
特許番号
US07241757B2

反応ノート

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