Bromide ion → HCID 135458024、化合物

HRID 229731

反応式

HRID 229731 の反応式
[CH3:1][CH:2]1[CH2:11][C:10]2[N:9]=[N:8][C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)=[CH:6][C:5]=2[C:4](=[O:22])[CH2:3]1.[Br-].C(=O)(O)[O-].[Na+]>C(OCC)(=O)C>[CH3:1][C:2]1[CH:3]=[C:4]([OH:22])[C:5]2[CH:6]=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=3)[N:8]=[N:9][C:10]=2[CH:11]=1

参加物

5

反応物 3

HCID 259Bromide ionHCID 516892Sodium BicarbonateHCID 100180127-methyl-3-(3-trifluoromethylphenyl)-7,8-dihydro-6H-cinnolin-5-one

生成物 1

HCID 135458024HCID 135458024、化合物収率 5.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒3 回

実験手順

To an ethyl acetate solution (1 mL) of 7-methyl-3-(3-trifluoromethylphenyl)-7,8-dihydro-6H-cinnolin-5-one (306 mg, 1.0 mmol) obtained in Example 66 was added cupuric bromide (446 mg, 2.0 mmol), followed by reaction under heating and refluxing for 8 hours, adding saturated sodium bicarbonate aqueous solution (2 mL) to the reaction liquid and extraction with ethyl acetate. To residue obtained after concentration of an organic layer under reduced pressure was added ethyl acetate (1 mL) and filtered off solid obtained to get an objective product (17 mg, 5.5%) as yellow solid.

後処理

  1. customfollowed by reaction
  2. temperatureunder heating
  3. temperaturerefluxing for 8 hours
  4. customTo residue obtained after concentration of an organic layer under reduced pressure
  5. filtrationfiltered off solid
  6. customobtained

出典と根拠

ORDレコード
ord-ff26126a4628438c9be7a02cf30b4270
出典データセット
uspto-grants-2009_07
特許番号
US07563893B2

関連ノート

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