2-Chlorobenzoxazole → HCID 58778947、化合物

HRID 1372668

反応式

HRID 1372668 の反応式
Cl[C:2]1[O:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[NH2:11][C:12]1[C:17]([Cl:18])=[CH:16][C:15]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])=[C:14]([F:25])[CH:13]=1>C1(C)C(C)=CC=CC=1>[O:3]1[C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=[C:2]1[NH:11][C:12]1[C:17]([Cl:18])=[CH:16][C:15]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])=[C:14]([F:25])[CH:13]=1

参加物

4

反応物 2

HCID 119862-ChlorobenzoxazoleHCID 17858807Ethyl 4-amino-5-chloro-2-fluorophenylacetate

生成物 1

HCID 58778947HCID 58778947、化合物収率 74%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

In xylene (4 ml), 2-chlorobenzoxazole (278 μl, 2.43 mmol) and ethyl (4-amino-5-chloro-2-fluorophenyl)acetate (512 mg, 2.21 mmol) were heated under reflux for 2 hours. After the reaction mixture was cooled to room temperature, the solvent was distilled off under reduced pressure. The residue was dissolved in ethyl acetate. The resulting solution was washed with a saturated aqueous solution of sodium bicarbonate, dried over anhydrous sodium sulfate, and distilled under reduced pressure to remove the solvent. The residue was purified by chromatography on a silica gel column, whereby from n-hexane/ethyl acetate (7:1, v/v) eluate fractions, ethyl (4-(2-benzoxazolyl)amino-5-chloro-2-fluorophenyl)acetate (570 mg, 74%) was obtained as a pale yellow solid.

後処理

  1. temperatureunder reflux for 2 hours
  2. distillationthe solvent was distilled off under reduced pressure
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washThe resulting solution was washed with a saturated aqueous solution of sodium bicarbonate
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationdistilled under reduced pressure
  7. customto remove the solvent
  8. customThe residue was purified by chromatography on a silica gel column, whereby from n-hexane/ethyl acetate (7:1

出典と根拠

ORDレコード
ord-4f7bd92e4e4c47be9740591b36e80cac
出典データセット
uspto-grants-2007_01
特許番号
US07157487B2

関連ノート

読み込み中…