Pyridine → HCID 135448269, 화합물

HRID 2217909노트

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HRID 2217909 반응식
[NH2:1][C:2](=[N:30][OH:31])[CH:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:18]=[CH:17][C:16]3[C:11](=[CH:12][CH:13]=[C:14]([Cl:29])[C:15]=3[NH:19][C:20](=[O:28])[CH2:21][CH:22]3[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]3)[N:10]=2)[CH2:5][CH2:4]1.N1C=CC=CC=1.C(C(CCCC)[CH2:41][O:42]C(Cl)=O)C>ClCCl>[Cl:29][C:14]1[C:15]([NH:19][C:20](=[O:28])[CH2:21][CH:22]2[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]2)=[C:16]2[C:11](=[CH:12][CH:13]=1)[N:10]=[C:9]([N:6]1[CH2:7][CH2:8][CH:3]([C:2]3[NH:1][C:41](=[O:42])[O:31][N:30]=3)[CH2:4][CH2:5]1)[CH:18]=[CH:17]2

참가 물질

5

반응물 3

HCID 1049PyridineHCID 627832-Ethylhexyl chloroformateHCID 86609749N-[2-[4-[Amino(hydroxyimino)methyl]-1-piperidinyl]-6-chloro-5-quinolinyl]-cyclohexaneacetamide

생성물 1

HCID 135448269HCID 135448269, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of N-[2-[4[amino(hydroxyimino)methyl]-1-piperidinyl]-6-chloro-5-quinolinyl]-cyclohexaneacetamide (example 102(a)) (0.1 g) and pyridine (0.02 mL) in dichloromethane (5 mL) at 0° C. was added 2-ethylhexylchloroformate (0.064 mL). After 10 minutes the reaction was allowed to warm to room temperature and was then stirred for 2 hours. The solvent was removed under vacuum and the resulting solid was transferred to a 10 mL microwave vial with isohexane (3 mL) and heated within a microwave at 140° C. for 20 minutes. The reaction mixture was filtered and the solid was taken up in boiling methanol (20 mL) and purified by Varian NH2 cartridge (methanol (50 mL) and then acetic acid:methanol 10:90 as eluant) to afford the title product (0.042 g).

후처리

  1. customThe solvent was removed under vacuum
  2. temperatureheated within a microwave at 140° C. for 20 minutes
  3. filtrationThe reaction mixture was filtered
  4. custompurified by Varian NH2 cartridge (methanol (50 mL)

출처 및 근거

ORD 기록
ord-a90cc9751bde4dec90c59d066ec12a4b
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07408065B2

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