Potassium Carbonate → HCID 58485966、化合物

HRID 1970862ノート

反応式

HRID 1970862 の反応式
[F:1][C:2]1[C:3]([F:12])=[CH:4][C:5]2[O:9][C:8](=[O:10])[NH:7][C:6]=2[CH:11]=1.Br[CH:14]([C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([N+:22]([O-:24])=[O:23])[CH:17]=1)[CH3:15].C(=O)([O-])[O-].[K+].[K+]>C(#N)C.CC(OC)(C)C>[F:1][C:2]1[C:3]([F:12])=[CH:4][C:5]2[O:9][C:8](=[O:10])[N:7]([CH:14]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([N+:22]([O-:24])=[O:23])[CH:17]=3)[CH3:15])[C:6]=2[CH:11]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 115356375,6-difluorobenzo[d]oxazol-2(3H)-oneHCID 229178381-(1-Bromoethyl)-3-nitrobenzene

生成物 1

HCID 58485966HCID 58485966、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 15413tert-Butyl methyl ether溶媒

反応条件

温度
60 °C

実験手順

500 mg (2.9 mmol) of 5,6-difluoro-3H-benzoxazol-2-one, 672 mg (2.9 mmol) of (1-bromoethyl)-3-nitrobenzene and 1.58 g (11.4 mmol) of potassium carbonate are suspended in 6 ml of acetonitrile, and the mixture is stirred at 60° C. for 6 h. The mixture is subsequently diluted with 30 ml of MTBE, washed with 3×20 ml of H2O, dried over sodium sulfate and evaporated to dryness. The crude product is purified by column chromatography on silica gel.

後処理

  1. washwashed with 3×20 ml of H2O
  2. dry with materialdried over sodium sulfate
  3. customevaporated to dryness
  4. customThe crude product is purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-dbe0198a2b494c43ad3adb416cd78886
出典データセット
uspto-grants-2013_04
特許番号
US08431572B2

反応ノート

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