Potassium Carbonate → HCID 10188544、化合物

HRID 1635111ノート

反応式

HRID 1635111 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-82c83b8e960b468c9cae69a495102481
出典データセット
uspto-grants-2003_01
特許番号
US06509333B2

反応ノート

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