Trifluoroacetic acid → HCID 21060031, 화합물

HRID 921946노트

반응식

HRID 921946 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 21060031HCID 21060031, 화합물수율 62.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-1d15aa6bae0344c7ba5e166c51504ed8
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09273057B2

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