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

HRID 353248ノート

反応式

HRID 353248 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 subtitle 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-8efa8896b30c49c487ad764f0aac41cd
出典データセット
uspto-grants-2004_06
特許番号
US06750243B1

反応ノート

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