Trifluoroacetic acid → Rac-2-methyl-3-phenyl-2,6-diazaspiro[3.5]nonan-1-one

HRID 1036733노트

반응식

HRID 1036733 반응식
[CH3:1][N:2]1[CH:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:4]2([CH2:16][CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12]2)[C:3]1=[O:24].C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:1][N:2]1[CH:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:4]2([CH2:16][CH2:15][CH2:14][NH:13][CH2:12]2)[C:3]1=[O:24]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 71060344Tert-butyl 2-methyl-1-oxo-3-phenyl-2,6-diazaspiro[3.5]nonane-6-carboxylate

생성물 1

HCID 71060408Rac-2-methyl-3-phenyl-2,6-diazaspiro[3.5]nonan-1-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution comprising tert-butyl 2-methyl-1-oxo-3-phenyl-2,6-diazaspiro[3.5]nonane-6-carboxylate (1.2 g, 3.63 mmol) and TFA (1.399 ml, 18.16 mmol) in DCM (20 ml) was stirred at RT for 4 days. The reaction mixture was concentrated in vacuo and the resulting crude product was dissolved with methanol (5 ml) and passed through a 10 g SCX-2 cartridge. The product was eluted with 2M NH3 in methanol (70 ml) and the relevant fractions were combined and concentrated in vacuo to afford the title compound as a yellow oil;

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutionthe resulting crude product was dissolved with methanol (5 ml)
  3. washThe product was eluted with 2M NH3 in methanol (70 ml)
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3de07fc0f22948709b9bab385a90bcb4
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546416B2

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