Trifluoroacetic acid → Isopropyl 4-aminopiperidine-1-carboxylate

HRID 448584

反応式

HRID 448584 の反応式
[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([NH:13]C(OC(C)(C)C)=O)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2].C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH:1]([O:4][C:5]([N:7]1[CH2:8][CH2:9][CH:10]([NH2:13])[CH2:11][CH2:12]1)=[O:6])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 597771674-Tert-butoxycarbonylamino-piperidine-1-carboxylic acid isopropyl ester

生成物 1

HCID 46941577Isopropyl 4-aminopiperidine-1-carboxylate収率 89.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 18a (3.26 g, 11.37 mmol) in 10 mL of DCM, was added TFA (5 mL, 64.9 mmol). The mixture was stirred at room temperature for 2 h and the solvent were evaporated. The residue was dissolved in DCM and a saturated solution of NaHCO3 and 1N NaOH were added until pH was 8. The layers were separated and the aqueous layer was extracted with 3:1 DCM:IPA (3×40 mL). The organic extracts were combined, dried, filtered and evaporated to afford 1.89 g (89%) of 18b.

後処理

  1. customthe solvent were evaporated
  2. dissolutionThe residue was dissolved in DCM
  3. additiona saturated solution of NaHCO3 and 1N NaOH were added until pH was 8
  4. customThe layers were separated
  5. extractionthe aqueous layer was extracted with 3:1 DCM
  6. customdried
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-99d07a368f414150bfa89fa12d747a27
出典データセット
uspto-grants-2013_07
特許番号
US08481731B2

関連ノート

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