Potassium Fluoride → [5-(4-{1-(4-Fluorophenyl)-3-[3-(4-fluorophenyl)-3-(tert-butyldimethylsilanyloxy)propyl]-4-oxoazetidin-2-yl}phenoxy)pentyl]trimethylammonium bromide

HRID 1725300ノート

反応式

HRID 1725300 の反応式
[Si:1]([O:8][CH:9]([C:31]1[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=1)[CH2:10][CH2:11][CH:12]1[CH:15]([C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=2)[N:14]([C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)[C:13]1=[O:30])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[F-].[K+].[Br-].[Br:41][CH:42]([CH2:49][CH3:50])[CH2:43][CH2:44][N+:45]([CH3:48])([CH3:47])[CH3:46]>C(#N)C>[Br-:41].[F:29][C:26]1[CH:25]=[CH:24][C:23]([N:14]2[C:13](=[O:30])[CH:12]([CH2:11][CH2:10][CH:9]([C:31]3[CH:32]=[CH:33][C:34]([F:37])=[CH:35][CH:36]=3)[O:8][Si:1]([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2])[CH:15]2[C:16]2[CH:21]=[CH:20][C:19]([O:22][CH2:50][CH2:49][CH2:42][CH2:43][CH2:44][N+:45]([CH3:48])([CH3:47])[CH3:46])=[CH:18][CH:17]=2)=[CH:28][CH:27]=1

参加物

5

反応物 3

HCID 522689Potassium FluorideHCID 22252045(3-Bromopentyl)-trimethylammonium bromideHCID 222520743-[3-(tert-Butyldimethylsilanyloxy)-3-(4-fluorophenyl)propyl]-1-(4-fluorophenyl)-4-(4-hydroxyphenyl)azetidin-2-one

生成物 1

HCID 22252089[5-(4-{1-(4-Fluorophenyl)-3-[3-(4-fluorophenyl)-3-(tert-butyldimethylsilanyloxy)propyl]-4-oxoazetidin-2-yl}phenoxy)pentyl]trimethylammonium bromide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

370 mg of 3-[3-(tert-butyldimethylsilanyloxy)-3-(4-fluorophenyl)propyl]-1-(4-fluorophenyl)-4-(4-hydroxyphenyl)azetidin-2-one are dissolved in 3 ml of absolute acetonitrile. 300 mg of KF.alumina (1.15 mol/100 g) and 375 mg of (3-bromopentyl)-trimethylammonium bromide are then added. The reaction mixture is stirred at room temperature overnight and then filtered. The mother liquor is concentrated using a rotary evaporator and the residue is purified using a 5 g SiO2 cartridge (dichloromethane/methanol 4:1). The product is obtained as an oil.

後処理

  1. filtrationfiltered
  2. concentrationThe mother liquor is concentrated
  3. customa rotary evaporator
  4. customthe residue is purified
  5. customThe product is obtained as an oil

出典と根拠

ORDレコード
ord-2a5c659f2d7d48cb9328ea51f58e2dd5
出典データセット
uspto-grants-2009_02
特許番号
US07488829B2

反応ノート

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