2-Amino-5-chloro-2'-fluorobenzophenone → HCID 23322779、化合物

HRID 279848

反応式

HRID 279848 の反応式
Cl.[CH3:2][C:3]1[NH:4]C=CN=1.[NH2:8][C:9]1[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][C:10]=1[C:11]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[F:19])=O.C(=O)(O)[O-:26].[Na+]>C(CN)O>[NH2:8][C:9]1[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][C:10]=1[C:11]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[F:19])=[N:4][CH2:3][CH2:2][OH:26]

参加物

5

反応物 3

HCID 699122-Amino-5-chloro-2'-fluorobenzophenoneHCID 516892Sodium BicarbonateHCID 5216292-Methylimidazole hydrochloride

生成物 1

HCID 23322779HCID 23322779、化合物

試薬・触媒・溶媒 1

HCID 700Ethanolamine溶媒

実験手順

A mixture of 40 g of 2-methylimidazole hydrochloride and of 90 g of 2-amino-5-chloro-2'-fluoro-benzophenone in 240 ml of ethanolamine is heated at 135° for 2 hours. After cooling, the reaction mixture is poured into an aqueous sodium bicarbonate solution. The mixture is extracted with ether, the organic phase is washed repeatedly with water and is dried over sodium sulphate, and the solvent is evaporated to dryness. The residual oil is chromatographed on a silica column, elution being carried out with a 50/50 mixture of cyclohexane and ethyl acetate.

後処理

  1. temperatureAfter cooling
  2. extractionThe mixture is extracted with ether
  3. washthe organic phase is washed repeatedly with water
  4. dry with materialis dried over sodium sulphate
  5. customthe solvent is evaporated to dryness
  6. customThe residual oil is chromatographed on a silica column, elution
  7. additionbeing carried out with a 50/50 mixture of cyclohexane and ethyl acetate

出典と根拠

ORDレコード
ord-eea19af2b3f74012a5225b25d3936404
出典データセット
uspto-grants-1986_05
特許番号
US04587245

関連ノート

読み込み中…