Potassium Carbonate → HCID 21942288、化合物

HRID 2216359ノート

反応式

HRID 2216359 の反応式
CS(O[CH2:6][C@H:7]1[C@@H:9]([CH2:10]OS(C)(=O)=O)[O:8]1)(=O)=O.[Br:16][C:17]1[CH:18]=[C:19]([CH:21]=[CH:22][CH:23]=1)[NH2:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Br:16][C:17]1[CH:18]=[C:19]([N:20]2[CH2:10][CH:9]3[O:8][CH:7]3[CH2:6]2)[CH:21]=[CH:22][CH:23]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 115623-BromoanilineHCID 86591773HCID 86591773、化合物

生成物 1

HCID 21942288HCID 21942288、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

A mixture of 5.4 g of cis-2,3-bis(methanesulfonyloxymethyl)oxirane, 2 ml of 3-bromoaniline, 4.3 g of anhydrous potassium carbonate and 30 ml of N,N-dimethylformamide was stirred under nitrogen atmosphere at 60° C. for 2 hours and at 110° C. for 2 hours. The reaction mixture was extracted with ethyl acetate-water, and the organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and then evaporated. The residue was purified by silica gel column chromatography with 5–10% ethyl acetate/hexane, to give 420 mg of the title compound.

後処理

  1. extractionThe reaction mixture was extracted with ethyl acetate-water
  2. washthe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customevaporated
  5. customThe residue was purified by silica gel column chromatography with 5–10% ethyl acetate/hexane

出典と根拠

ORDレコード
ord-0cb2c59eb93244c78d57d6d38bed98fc
出典データセット
uspto-grants-2006_09
特許番号
US07112593B2

反応ノート

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