1-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acid → HCID 21906386, 화합물

HRID 988600노트

반응식

HRID 988600 반응식
[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

참가 물질

5

반응물 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

생성물 1

HCID 21906386HCID 21906386, 화합물수율 18%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2b7d61efcc6b4341a4d1726f2d2a9ea5
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06635657B1

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