Triphenylphosphine → 3-(4-(Trifluoromethyl)benzamido)propyloxyphenyl benzoate

HRID 377732

反応式

HRID 377732 の反応式
[C:1]([O:9][C:10]1[CH:15]=[C:14](C)[C:13](O)=[C:12](CC)[CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:20][C:21]([F:36])([F:35])[C:22]1[CH:34]=[CH:33][C:25]([C:26]([NH:28][CH2:29][CH2:30][CH2:31][OH:32])=[O:27])=[CH:24][CH:23]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C>O1CCCC1>[C:1]([O:9][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:15]=1[O:32][CH2:31][CH2:30][CH2:29][NH:28][C:26](=[O:27])[C:25]1[CH:33]=[CH:34][C:22]([C:21]([F:35])([F:36])[F:20])=[CH:23][CH:24]=1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 220068303-(4-Trifluoromethylbenzamido)propan-1-olHCID 232824092-Ethyl-6-methyl-4-benzoyloxyphenol

生成物 1

HCID 867544953-(4-(Trifluoromethyl)benzamido)propyloxyphenyl benzoate収率 90%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a mixture of 0.5 g of crude 3-ethyl-4-hydroxy-5-methylphenyl benzoate, 0.48 g of 3-(4-(trifluoromethyl)benzamido)propan-1-ol, 0.54 g of triphenylphosphine and 10 ml of tetrahydrofuran was added dropwise a solution of 0.41 g of diisopropylazodicarboxylate dissolved in 2 ml of tetrahydrofuran, while stirring at room temperature. After stirring at room temperature for 24 hours, the reaction mixture was concentrated under reduced pressure to give a residue. The residue was subjected to silica gel chromatography, which afforded 0.87 g of 3-ethyl-5-methyl-4-(3-(4-(trifluromethyl)benzamido)propyloxyphenyl benzoate (90% yield).

後処理

  1. stirringAfter stirring at room temperature for 24 hours
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customto give a residue

出典と根拠

ORDレコード
ord-e0d9a0333a1c4cfda6efcf4fd2422423
出典データセット
uspto-grants-2000_02
特許番号
US06028100

関連ノート

読み込み中…