Phthalic Anhydride → HCID 178463969、化合物

HRID 25619

反応式

HRID 25619 の反応式
OO.NC(N)=[O:5].C1(=O)OC(=O)C2=CC=CC=C12.[C:18]([Si:22]([CH3:56])([CH3:55])[O:23][CH2:24][CH2:25][N:26]([CH2:53][CH3:54])[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][C@H:32]1[CH2:37][CH2:36][C@H:35]([N:38]([CH3:52])[S:39]([C:42]2[CH:47]=[CH:46][C:45]([C:48]([F:51])([F:50])[F:49])=[CH:44][CH:43]=2)(=[O:41])=[O:40])[CH2:34][CH2:33]1)([CH3:21])([CH3:20])[CH3:19]>C(Cl)Cl>[C:18]([Si:22]([CH3:55])([CH3:56])[O:23][CH2:24][CH2:25][N:26]([CH2:53][CH3:54])[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][C@H:32]1[CH2:33][CH2:34][C@H:35]([N+:38]([O-:5])([CH3:52])[S:39]([C:42]2[CH:47]=[CH:46][C:45]([C:48]([F:50])([F:51])[F:49])=[CH:44][CH:43]=2)(=[O:41])=[O:40])[CH2:36][CH2:37]1)([CH3:19])([CH3:20])[CH3:21]

参加物

5

反応物 3

HCID 6811Phthalic AnhydrideHCID 31294Carbamide PeroxideHCID 178463970HCID 178463970、化合物

生成物 1

HCID 178463969HCID 178463969、化合物収率 30.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

175 mg (1.86 mmol) H2O2-Urea adduct suspended in 2 ml CH2Cl2 were treated with 137 mg (0.9 mmol) phthalic anhydride. After stirring at RT for 15 min to this mixture was added 500 mg (8.4 mmol) crude trans-N-[4-(5-{[2-(tert-Butyl-dimethyl-silanyloxy)-ethyl]-ethyl-amino}-pentyl)-cyclohexyl]-N-methyl-4-trifluoromethyl-benzenesulfonamide in 3 ml CH2Cl2 and the solution was stirred at RT. The mixture was washed with an aqueous solution of NaHCO3, the organic phase was washed with brine and dried over Na2SO4.348 mg crude trans-N-[4-(5-{[2-(tert-Butyl-dimethyl-silanyloxy)-ethyl]-ethyl-amino}-pentyl)-cyclohexyl]-N-methyl-4-trifluoromethyl-benzenesulfonamide N-oxide were isolated as colorless oil.

後処理

  1. stirringthe solution was stirred at RT
  2. washThe mixture was washed with an aqueous solution of NaHCO3
  3. washthe organic phase was washed with brine
  4. dry with materialdried over Na2SO4

出典と根拠

ORDレコード
ord-7b410dd5c7b243e7b07af3012a0d8595
出典データセット
uspto-grants-2005_02
特許番号
US06858651B2

関連ノート

読み込み中…