Sodium Thiosulfate → HCID 59443055、化合物

HRID 1959125ノート

反応式

HRID 1959125 の反応式
C1C=C[NH+]=CC=1.[Br:7][Br-]Br.[Cl:10][C:11]1[CH:20]=[C:19]2[C:14]([C:15]([C:23]3[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=3)=[CH:16][C:17]([CH3:22])([CH3:21])[O:18]2)=[CH:13][CH:12]=1.S([O-])([O-])(=O)=S.[Na+].[Na+]>ClCCl>[Br:7][C:16]1[C:17]([CH3:21])([CH3:22])[O:18][C:19]2[C:14]([C:15]=1[C:23]1[CH:24]=[CH:25][C:26]([F:29])=[CH:27][CH:28]=1)=[CH:13][CH:12]=[C:11]([Cl:10])[CH:20]=2

参加物

4

反応物 2

HCID 24477Sodium ThiosulfateHCID 594429257-Chloro-4-(4-fluorophenyl)-2,2-dimethyl-2h-chromen

生成物 1

HCID 59443055HCID 59443055、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Pyridinium bromide perbromide (1.00 g) was added to a solution of 7-chloro-4-(4-fluorophenyl)-2,2-dimethyl-2H-chromen (a compound obtained in Reference Example 5(3); 1.00 g) in dichloromethane (15 mL) under ice-cooling and the mixture was stirred at room temperature for 1.5 hours. The reaction mixture was poured into a 15% aqueous solution of sodium thiosulfate and extracted with ethyl acetate. The organic layer was washed successively with a saturated solution of sodium bicarbonate and brine, dried over sodium sulfate and concentrated in vacuo. The resultant residue was purified by column chromatography on silica gel (Solvent: n-hexane/chloroform=100/0 to 95/5) to give the titled compound (1.26 g) as a colorless powder.

後処理

  1. customobtained in Reference Example 5(3)
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed successively with a saturated solution of sodium bicarbonate and brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resultant residue was purified by column chromatography on silica gel (Solvent: n-hexane/chloroform=100/0 to 95/5)

出典と根拠

ORDレコード
ord-d4df6ade9bfa4737a5e50ba2ce8a0512
出典データセット
uspto-grants-2013_04
特許番号
US08410166B2

反応ノート

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