Potassium Carbonate → HCID 10188544、化合物

HRID 273284ノート

反応式

HRID 273284 の反応式
[CH3:1][CH:2]([CH3:28])[CH2:3][C@H:4]([C:20]1([C:25]([NH2:27])=[O:26])[CH2:24][CH:23]=[CH:22][CH2:21]1)[C:5](=[O:19])[NH:6][CH:7]1[C:13](=[O:14])[NH:12][C:11]2[CH:15]=[CH:16][CH:17]=[CH:18][C:10]=2[CH2:9][CH2:8]1.C([O-])([O-])=O.[K+].[K+].[F:35][C:36]1[CH:50]=[CH:49][CH:48]=[CH:47][C:37]=1[O:38][C:39]1[CH:40]=[C:41]([CH:44]=[CH:45][CH:46]=1)[CH2:42]Br>CC#N>[F:35][C:36]1[CH:50]=[CH:49][CH:48]=[CH:47][C:37]=1[O:38][C:39]1[CH:40]=[C:41]([CH:44]=[CH:45][CH:46]=1)[CH2:42][N:12]1[C:13](=[O:14])[CH:7]([NH:6][C:5]([CH:4]([C:20]2([C:25]([NH2:27])=[O:26])[CH2:21][CH:22]=[CH:23][CH2:24]2)[CH2:3][CH:2]([CH3:28])[CH3:1])=[O:19])[CH2:8][CH2:9][C:10]2[CH:18]=[CH:17][CH:16]=[CH:15][C:11]1=2

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 27374543-(2-Fluorophenoxy)benzyl BromideHCID 59033282HCID 59033282、化合物

生成物 1

HCID 10188544HCID 10188544、化合物収率 77.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 20 (11 mg) in CH3CN (2 mL) was added K2CO3 (8 mg) and 3-(2-fluorophenoxy)benzyl bromide 22 (12 mg). The reaction mixture was stirred at rt for 20 hrs before the solvent was removed under pressure. The crude product was purified by flash chromatography to give compound 23 (77%, 13 mg). 1H NMR (300 MHz, CDCl3) 7.32-6.80 (m, 12H), 5.72 (m, 1H), 5.58 (m, 1H), 5.34 (d, 1H), 4.72 (d, 1H), 4.48 (m, 1H), 3.18 (m, 1H), 2.70-2.20 (m, 8H), 1.95-1.78 (m, 2H), 1.42 (m, 1H), 1.12 (m, 1H), 0.92-0.80 (q, 6H); MS [M+H]+ 584.

後処理

  1. customwas removed under pressure
  2. customThe crude product was purified by flash chromatography

出典と根拠

ORDレコード
ord-99ee983399fe45efa6c5b51103f94b8e
出典データセット
uspto-grants-2008_11
特許番号
US07456278B2

反応ノート

読み込み中…