Magnesium Bromide → HCID 89692873、化合物

HRID 1481844ノート

反応式

HRID 1481844 の反応式
C[O:2][C:3]1[C:8]([C:9](=[O:20])[NH:10][CH2:11][CH2:12][CH2:13][N:14]2[CH2:18][CH2:17][CH2:16][C:15]2=[O:19])=[CH:7][C:6]([NH:21][C:22]([C:24]2[N:25]=[C:26]([CH:29]3[CH2:31][CH2:30]3)[O:27][CH:28]=2)=[O:23])=[C:5]([N:32]2[CH2:37][CH2:36][N:35]([C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=3[CH3:44])[CH2:34][CH2:33]2)[CH:4]=1.[Br-].[Mg+2].[Br-]>N1C=CC=CC=1>[OH:2][C:3]1[C:8]([C:9](=[O:20])[NH:10][CH2:11][CH2:12][CH2:13][N:14]2[CH2:18][CH2:17][CH2:16][C:15]2=[O:19])=[CH:7][C:6]([NH:21][C:22]([C:24]2[N:25]=[C:26]([CH:29]3[CH2:30][CH2:31]3)[O:27][CH:28]=2)=[O:23])=[C:5]([N:32]2[CH2:33][CH2:34][N:35]([C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=3[CH3:44])[CH2:36][CH2:37]2)[CH:4]=1

参加物

4

反応物 2

HCID 82241Magnesium BromideHCID 71667528HCID 71667528、化合物

生成物 1

HCID 89692873HCID 89692873、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
130 °C

実験手順

To a solution of 2-cyclopropyl-oxazole-4-carboxylic acid [4-methoxy-5-[3-(2-oxo-pyrrolidin-1-yl)-propylcarbamoyl]-2-(4-o-tolyl-piperazin-1-yl)-phenyl]-amide 2c (40.0 mg, 0.067 mmol) in pyridine (5.0 mL) was added magnesium bromide (49.0 mg, 0.268 mmol). The reaction was stirred at 130° C. for 16 h. Cooled, concentrated and the crude 2d was dissolved in methanol/water mixture and purified on preparative HPLC using methanol/water as eluent.

後処理

  1. temperatureCooled
  2. concentrationconcentrated
  3. dissolutionthe crude 2d was dissolved in methanol/water mixture
  4. custompurified on preparative HPLC

出典と根拠

ORDレコード
ord-bf15a91e4c4c487eb584c1a6cd9b8096
出典データセット
uspto-grants-2016_08
特許番号
US09409897B2

反応ノート

読み込み中…