Sodium Thiosulfate → HCID 59443055, 화합물

HRID 1959125노트

반응식

HRID 1959125 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 59443055HCID 59443055, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d4df6ade9bfa4737a5e50ba2ce8a0512
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08410166B2

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