ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Bromotrimethylsilane → 1-Phosphonomethyl-7-trifluoromethyl[1,2,4]triazolo[4,3-a]quinoxalin-4(5H)-one

HRID 744026
ノート
印刷プレビュー

反応式

HRID 744026 の反応式
Br[Si](C)(C)C.C([O:8][P:9]([CH2:14][C:15]1[N:19]2[C:20]3[C:25]([NH:26][C:27](=[O:28])[C:18]2=[N:17][N:16]=1)=[CH:24][C:23]([C:29]([F:32])([F:31])[F:30])=[CH:22][CH:21]=3)([O:11]CC)=[O:10])C>C(#N)C>[P:9]([CH2:14][C:15]1[N:19]2[C:20]3[C:25]([NH:26][C:27](=[O:28])[C:18]2=[N:17][N:16]=1)=[CH:24][C:23]([C:29]([F:31])([F:30])[F:32])=[CH:22][CH:21]=3)([OH:10])([OH:11])=[O:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 76113BromotrimethylsilaneHCID 194214281-[(Diethoxyphosphoryl)methyl]-7-trifluoromethyl[1,2,4]triazolo[4,3-a]quinoxalin-4(5H)-one

生成物 1

HCID 98196891-Phosphonomethyl-7-trifluoromethyl[1,2,4]triazolo[4,3-a]quinoxalin-4(5H)-one収率 70%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
40 °C

実験手順

Bromotrimethylsilane (0.75 ml, 5.8 mmol) was added to a suspension of 1-[(diethoxyphosphoryl)methyl]-7-trifluoromethyl[1,2,4]triazolo[4,3-a]quinoxalin-4(5H)-one (315 mg, 0.78 mmol) in 15 ml of dry acetonitrile in a flame-dried flask under nitrogen, and the resulting solution was stirred overnight at 40° C. After evaporation to dryness, the residue was stirred with 25 ml of water for 1 h. Then the water was removed under reduced pressure by azeotropic distillation with 1-propanol, and the residue was crystallized by trituration with a mixture of ether and ethanol followed by light petroleum. The solid was recrystallized from water, and dried in vacuo to give 189 mg (70%) of the title compound, m.p.>290° C. dec. (DSC); 1H-NMR (DMSO-d6): δ 3.96 (d, 2H), 7.64 (d, 1H), 7.69 (s, 1H), 8.47 (d, 1H), 12.28 (s, 1H); IR (KBr): 1712 cm-1 ; MS (FAB): m/e 349 (MH+).

後処理

  1. customAfter evaporation to dryness
  2. stirringthe residue was stirred with 25 ml of water for 1 h
  3. customThen the water was removed under reduced pressure by azeotropic distillation with 1-propanol
  4. customthe residue was crystallized by trituration with a mixture of ether and ethanol
  5. customThe solid was recrystallized from water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-4826525391004de588074152ecf4e42a
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05559106

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート