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Potassium Carbonate → 4-[3-Difluoromethoxy-2-methoxy-6-(1-oxo-indan-4-yl)-phenoxymethyl]-benzenesulfonamide

HRID 2171074
ノート
印刷プレビュー

反応式

HRID 2171074 の反応式
[F:1][CH:2]([F:23])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:18]=[CH:17][CH:16]=[C:15]3[C:11]=2[CH2:12][CH2:13][C:14]3=[O:19])=[C:6]([OH:20])[C:5]=1[O:21][CH3:22].C(=O)([O-])[O-].[K+].[K+].Br[CH2:31][C:32]1[CH:37]=[CH:36][C:35]([S:38]([NH2:41])(=[O:40])=[O:39])=[CH:34][CH:33]=1>C(#N)C>[F:1][CH:2]([F:23])[O:3][C:4]1[C:5]([O:21][CH3:22])=[C:6]([C:7]([C:10]2[CH:18]=[CH:17][CH:16]=[C:15]3[C:11]=2[CH2:12][CH2:13][C:14]3=[O:19])=[CH:8][CH:9]=1)[O:20][CH2:31][C:32]1[CH:33]=[CH:34][C:35]([S:38]([NH2:41])(=[O:40])=[O:39])=[CH:36][CH:37]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 131545004-BromomethylbenzenesulfonamideHCID 674685304-(4-(Difluoromethoxy)-2-hydroxy-3-methoxyphenyl)-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 674618654-[3-Difluoromethoxy-2-methoxy-6-(1-oxo-indan-4-yl)-phenoxymethyl]-benzenesulfonamide収率 33%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile
溶媒

反応条件

温度
80 °C

実験手順

To a stirring solution of 4-(4-(difluoromethoxy)-2-hydroxy-3-methoxyphenyl)-2,3-dihydro-1H-inden-1-one (80 mg, 0.25 mmol) in acetonitrile (10 mL), was added potassium carbonate (104 mg, 0.75 mmol) and 4-bromomethyl-benzenesulfonamide (125 mg, 0.5 mmol) and the resultant reaction mixture was heated to 80° C. for 16 h. The reaction mixture was cooled to RT and filtered through celite and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, 0-70° A) ethyl acetate in pet ether) to afford title compound as a solid (40 mg, 33%).

後処理

  1. customthe resultant reaction mixture
  2. temperatureThe reaction mixture was cooled to RT
  3. filtrationfiltered through celite
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by column chromatography (silica gel, 0-70° A) ethyl acetate in pet ether)

出典と根拠

ORDレコード
ord-af2d3ac40f794158920379fece67f5be
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051290B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート