Hydrochloric Acid → HCID 57656563、化合物

HRID 911594ノート

反応式

HRID 911594 の反応式
Cl.O1CCOCC1.C(OC([NH:15][CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23](=[O:29])[CH2:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[CH:19][C:18]=1[F:30])=O)(C)(C)C.C([O-])(O)=O.[Na+]>ClCCl>[CH3:26][C:25]([CH3:28])([CH3:27])[CH2:24][C:23]([C:20]1[CH:21]=[CH:22][C:17]([CH2:16][NH2:15])=[C:18]([F:30])[CH:19]=1)=[O:29]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 57656601HCID 57656601、化合物

生成物 1

HCID 57656563HCID 57656563、化合物収率 101.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Add 4N hydrogen chloride in dioxane (5.5 mL, 22 mmol) to a solution of N-(tert-butoxycarbonyl)-4-(3,3-dimethyl-butyryl)-2-fluoro-benzylamine (600 mg, 1.85 mmol) in dichloromethane (22 mL) and stir for 6.5 h. Concentrate in vacuo and wash the solid obtained with diethyl ether. Suspend the solid into saturated aqueous NaHCO3 and stir for 30 min. Extract the aqueous phase twice with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo to obtain the title compound as an oil (420 mg, 99%).

後処理

  1. concentrationConcentrate in vacuo
  2. washwash the solid
  3. customobtained with diethyl ether
  4. stirringstir for 30 min
  5. extractionExtract the aqueous phase twice with EtOAc
  6. dry with materialDry the combined organic extracts over Na2SO4
  7. filtrationfilter
  8. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-1d008622a3b1413d9eea17401871c20d
出典データセット
uspto-grants-2011_09
特許番号
US08022062B2

反応ノート

読み込み中…