Trifluoroacetic acid → HCID 21060031、化合物

HRID 921946ノート

反応式

HRID 921946 の反応式
Cl.[CH2:2]1[C:6]2([CH2:11][CH2:10][N:9](C(OC(C)(C)C)=O)[CH2:8][CH2:7]2)[CH2:5][CH2:4][NH:3]1.[CH3:19][C:20](OC(C)=O)=[O:21].C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH2:2]1[C:6]2([CH2:7][CH2:8][NH:9][CH2:10][CH2:11]2)[CH2:5][CH2:4][N:3]1[C:20](=[O:21])[CH3:19]

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 7918Acetic AnhydrideHCID 66833979tert-Butyl 2,8-diazaspiro[4.5]decane-8-carboxylate--hydrogen chloride (1/1)

生成物 1

HCID 21060031HCID 21060031、化合物収率 62.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A stirred solution of tert-butyl 2,8-diazaspiro[4.5]decane-8-carboxylate hydrochloride (400 mg, 1.445 mmol) in DCM (5 mL) was treated with TEA (0.604 mL, 4.34 mmol), followed by Ac2O (0.164 mL, 1.734 mmol), stirred at room temperature for 2 h. To this reaction mixture was added TFA (2.115 mL, 27.5 mmol) and stirred at room temperature for h. Concentrated under reduced pressure to obtain crude material which purified by SCX cartridge, loading with MeOH, washed with additional MeOH. Product was recovered eluting with 2M NH3 in MeOH. Solvent evaporation gave 1-(2,8-diazaspiro[4.5]decan-2-yl)ethanone (165 mg)

後処理

  1. stirringstirred at room temperature for h
  2. concentrationConcentrated under reduced pressure
  3. customto obtain crude material which
  4. custompurified by SCX cartridge
  5. washwashed with additional MeOH
  6. customProduct was recovered
  7. washeluting with 2M NH3 in MeOH
  8. customSolvent evaporation

出典と根拠

ORDレコード
ord-1d15aa6bae0344c7ba5e166c51504ed8
出典データセット
uspto-grants-2016_03
特許番号
US09273057B2

反応ノート

読み込み中…