HCID 59605970、化合物 → (4-Methylpiperidin-4-yl)(pyrrolidin-1-yl)methanone

HRID 1945493ノート

反応式

HRID 1945493 の反応式
C(OC([N:8]1[CH2:13][CH2:12][C:11]([CH3:21])([C:14]([N:16]2[CH2:20][CH2:19][CH2:18][CH2:17]2)=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C>C(O)(C(F)(F)F)=O.C(Cl)Cl.O>[CH3:21][C:11]1([C:14]([N:16]2[CH2:20][CH2:19][CH2:18][CH2:17]2)=[O:15])[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1

参加物

5

反応物 1

HCID 59605970HCID 59605970、化合物

生成物 1

HCID 24728852(4-Methylpiperidin-4-yl)(pyrrolidin-1-yl)methanone収率 99.9%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of 4-methyl-4-(pyrrolidine-1-carbonyl)piperidine-1-carboxylic acid tert-butyl ester (296 mg, 1.0 mmol) in TFA (5 mL), DCM (5 mL) and water (0.1 mL) was stirred at room temperature for 2 hours and then concentrated under reduced pressure. The residue was taken up in MeOH and loaded onto an Isolute® SCX-2 cartridge (10 g). The cartridge was washed with MeOH and the desired product was eluted with 2M NH3 in MeOH. The solvents were removed to give the desired product as a white solid (196 mg, 66%). LCMS (Method A): RT 0.31 min; [M+H]+ 197

後処理

  1. concentrationconcentrated under reduced pressure
  2. washThe cartridge was washed with MeOH
  3. washthe desired product was eluted with 2M NH3 in MeOH
  4. customThe solvents were removed

出典と根拠

ORDレコード
ord-e9fa50f03ccb4474a83d7c8d5b11b311
出典データセット
uspto-grants-2013_03
特許番号
US08394796B2

反応ノート

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