Pyridine → HCID 135448269、化合物

HRID 2217909ノート

反応式

HRID 2217909 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 135448269HCID 135448269、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a90cc9751bde4dec90c59d066ec12a4b
出典データセット
uspto-grants-2008_08
特許番号
US07408065B2

反応ノート

読み込み中…