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

HRID 921941ノート

反応式

HRID 921941 の反応式
[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]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 58893162HCID 58893162、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7e9e8980a06c47dbbd3363eaf04aef7a
出典データセット
uspto-grants-2016_03
特許番号
US09273057B2

反応ノート

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