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Triethylamine → 1-(N,N'-Bis(tert-butoxycarbonyl)carbamimidoyl)piperidine-4-carboxylic acid

HRID 1053814
ノート
印刷プレビュー

反応式

HRID 1053814 の反応式
FC(F)(F)C(O)=O.[NH:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=[O:15])[CH2:10][CH2:9]1.C(N(CC)CC)C.[CH3:24][C:25]([O:28][C:29]([NH:31][C:32](N1C=CC=N1)=[N:33][C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35])=[O:30])([CH3:27])[CH3:26]>CO>[CH3:27][C:25]([O:28][C:29]([NH:31][C:32]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=[O:15])[CH2:10][CH2:9]1)=[N:33][C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35])=[O:30])([CH3:24])[CH3:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 4428040N,N'-Bis(tert-butoxycarbonyl)-1H-pyrazole-1-carboxamidineHCID 90014521Piperidine-4-carboxylic acid trifluoroacetate salt

生成物 1

HCID 1317362991-(N,N'-Bis(tert-butoxycarbonyl)carbamimidoyl)piperidine-4-carboxylic acid収率 76%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of piperidine-4-carboxylic acid trifluoroacetate salt (0.20 g, 0.82 mmol) in methanol (10 mL), triethylamine (0.20 mL, 1.6 mmol) and N,N′-bis{[(2-methyl-2-propanyl)oxy]carbonyl}-1H-pyrazole-1-carboximidamide (0.30 g, 0.98 mmol) was added and the reaction mixture stirred at room temperature for 18 h. The solvent was evaporated under reduced pressure and the resulting residue dissolved in ethyl acetate and washed with brine. The organic layer was dried and concentrated to dryness to obtain the title compound (200 mg, 76%) as a white solid.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe resulting residue dissolved in ethyl acetate
  3. washwashed with brine
  4. customThe organic layer was dried
  5. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-83991b3e84934ade90b87135aac581d9
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394250B2

反応ノート

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