1-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acid → HCID 21906386、化合物

HRID 1247031ノート

反応式

HRID 1247031 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9](=[O:17])[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[NH2:16])=[N:6][CH:7]=1.[C:18]([N:25]1[CH2:33][CH2:32][CH:28]([C:29](O)=[O:30])[CH2:27][CH2:26]1)([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19].Cl.CN(C)CCCN=C=NCC>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9](=[O:17])[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[NH:16][C:29]([CH:28]2[CH2:32][CH2:33][N:25]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:26][CH2:27]2)=[O:30])=[N:6][CH:7]=1

参加物

5

反応物 3

HCID 3928711-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 219063812-amino-N-(5-chloropyridin-2-yl)benzamide

生成物 1

HCID 21906386HCID 21906386、化合物収率 18%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of N-(5-chloropyridin-2-yl)-2-aminobenzamide (0.5 g, 1.79 mmol) and Boc-isonipecotic acid (0.41 g, 1.79 mmol) in N,N-dimethylformamide (30 mL) was added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.69 g, 3.58 mmol). After stirring for 15 h, the solvent was removed in vacuo. The residue was partitioned between ethyl acetate and water, and the layers separated. The organic phase was washed with saturated aqueous sodium chloride, dried (magnesium sulfate), filtered, and concentrated in vacuo. The solid was suspended in ether, sonicated, and filtered to give 0.147 g (18%) of a tan solid.

後処理

  1. customthe solvent was removed in vacuo
  2. customThe residue was partitioned between ethyl acetate and water
  3. customthe layers separated
  4. washThe organic phase was washed with saturated aqueous sodium chloride
  5. dry with materialdried (magnesium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customsonicated
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-9edc2d5d47dc4001b88579a444a97950
出典データセット
uspto-grants-2006_10
特許番号
US07129245B2

反応ノート

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