Trifluoroacetic acid → 2-Methyl-2,8-diazaspiro[4.5]decan-1-one

HRID 921941노트

반응식

HRID 921941 반응식
[CH3:1][N:2]1[CH2:6][CH2:5][C:4]2([CH2:11][CH2:10][N:9](C(OC(C)(C)C)=O)[CH2:8][CH2:7]2)[C:3]1=[O:19].C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:1][N:2]1[CH2:6][CH2:5][C:4]2([CH2:11][CH2:10][NH:9][CH2:8][CH2:7]2)[C:3]1=[O:19]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 58893162HCID 58893162, 화합물

생성물 1

HCID 3270242-Methyl-2,8-diazaspiro[4.5]decan-1-one수율 89.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl 2-methyl-1-oxo-2,8-diazaspiro[4.5]decane-8-carboxylate (315 mg, 1.174 mmol) in DCM (5 mL) was added TFA (1.718 mL, 22.30 mmol) and the mixture was stirred at room temperature for 2 h. The reaction was concentrated under reduced pressure to obtain crude and purified by SCX cartridge, loading with MeOH, washed with additional MeOH. Product was recovered eluting with 2M NH3 in MeOH. Solvent evaporation gave 2-methyl-2,8-diazaspiro[4.5]decan-1-one (177 mg).

후처리

  1. concentrationThe reaction was concentrated under reduced pressure
  2. customto obtain crude
  3. custompurified by SCX cartridge
  4. washwashed with additional MeOH
  5. customProduct was recovered
  6. washeluting with 2M NH3 in MeOH
  7. customSolvent evaporation

출처 및 근거

ORD 기록
ord-7e9e8980a06c47dbbd3363eaf04aef7a
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09273057B2

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