Potassium Bicarbonate → 3-Bromo-5-(4-(2,3-di-p-tolyl-7,8-dihydropyrido[2,3-b]pyrazin-5(6H)-yl)butyl)-4,5-dihydroisoxazole

HRID 517915ノート

反応式

HRID 517915 の反応式
[CH2:1]([N:7]1[C:12]2=[N:13][C:14]([C:24]3[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=3)=[C:15]([C:17]3[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=3)[N:16]=[C:11]2[CH2:10][CH2:9][CH2:8]1)[CH2:2][CH2:3][CH2:4][CH:5]=[CH2:6].C(=O)([O-])O.[K+].[Br:36][C:37](Br)=[N:38][OH:39]>CCOC(C)=O>[Br:36][C:37]1[CH2:6][CH:5]([CH2:4][CH2:3][CH2:2][CH2:1][N:7]2[C:12]3=[N:13][C:14]([C:24]4[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=4)=[C:15]([C:17]4[CH:18]=[CH:19][C:20]([CH3:23])=[CH:21][CH:22]=4)[N:16]=[C:11]3[CH2:10][CH2:9][CH2:8]2)[O:39][N:38]=1

参加物

5

反応物 3

HCID 516893Potassium BicarbonateHCID 27632191-bromo-N-hydroxymethanecarbonimidoyl bromideHCID 896901775-(Hex-5-enyl)-2,3-dip-tolyl-5,6,7,8-tetrahydropyrido[2,3-b]pyrazine2 回

生成物 1

HCID 896903823-Bromo-5-(4-(2,3-di-p-tolyl-7,8-dihydropyrido[2,3-b]pyrazin-5(6H)-yl)butyl)-4,5-dihydroisoxazole

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

A mixture comprising 5-(hex-5-enyl)-2,3-di-p-tolyl-5,6,7,8-tetrahydropyrido[2,3-b]pyrazine (Intermediate H) (3.98 g, 10 mmol) and potassium hydrogen carbonate (5.01 g, 50.0 mmol) in EtOAc (50 ml) was treated dropwise with dibromoformaldoxime (6.08 g, 30.0 mmol) in EtOAc (50 ml) over 2 hours. The mixture was stirred at room temperature overnight and then filtered. The filtrate was washed with 1H HCl, water, brine and dried by passing through a phase separator. The solvent was removed under reduced pressure to afford the titled compound which was used without further purification.

後処理

  1. filtrationfiltered
  2. washThe filtrate was washed with 1H HCl, water, brine
  3. customdried
  4. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-e449091dabbd4134ac8d36a5a41f4c7b
出典データセット
uspto-grants-2015_08
特許番号
US09115129B2

反応ノート

読み込み中…