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

Tetrabutylammonium borohydride → HCID 67070116、化合物

HRID 1924445
ノート
印刷プレビュー

反応式

HRID 1924445 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]([NH:5][C:6]1[CH:15]=[CH:14][C:9]([C:10]([O:12][CH3:13])=[O:11])=[CH:8][CH:7]=1)=O.[BH4-].C([N+](CCCC)(CCCC)CCCC)CCC>C(Cl)Cl>[F:1][C:2]([F:16])([F:17])[CH2:3][NH:5][C:6]1[CH:7]=[CH:8][C:9]([C:10]([O:12][CH3:13])=[O:11])=[CH:14][CH:15]=1
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 169536Tetrabutylammonium borohydrideHCID 786481Methyl 4-[(trifluoroacetyl)amino]benzoate

生成物 1

HCID 67070116HCID 67070116、化合物収率 37%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
50 °C

実験手順

step c—A vial was charged with 122 (1.0 g, 4.05 mmol) and DCM (15 mL) then tetrabutylammonium borohydride was added. The vial was capped and heated overnight in an oil bath at 50° C. The reaction mixture was cooled to RT and the DCM was evaporated. HOAc was added dropwise until H2 evolution ceased. The solvents were evaporated and toluene was added. The mixture was made basic with dilute NaHCO3, extracted with EtOAc, dried (MgSO4), filtered and evaporated. The resulting solid was recrystallized from hexane to afford 0.349 g of methyl 4-(2,2,2-trifluoro-ethylamino)-benzoate (124)

後処理

  1. customThe vial was capped
  2. temperatureThe reaction mixture was cooled to RT
  3. customthe DCM was evaporated
  4. additionHOAc was added dropwise until H2 evolution
  5. customThe solvents were evaporated
  6. additiontoluene was added
  7. extractionextracted with EtOAc
  8. dry with materialdried (MgSO4)
  9. filtrationfiltered
  10. customevaporated
  11. customThe resulting solid was recrystallized from hexane

出典と根拠

ORDレコード
ord-82b526c065fe430eb245d7812cede589
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08178547B2

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