Tetrahydrofuran → HCID 135430203, 화합물

HRID 2217910노트

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HRID 2217910 반응식
[NH2:1][C:2](=[N:30]O)[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.[C:32](N1C=CN=C1)(N1C=CN=C1)=[S:33].[O:44]1CCCC1>C(Cl)(Cl)Cl.CO>[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:32](=[O:44])[S:33][N:30]=3)[CH2:4][CH2:5]1)[CH:18]=[CH:17]2

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 802641,1'-ThiocarbonyldiimidazoleHCID 86609749N-[2-[4-[Amino(hydroxyimino)methyl]-1-piperidinyl]-6-chloro-5-quinolinyl]-cyclohexaneacetamide

생성물 1

HCID 135430203HCID 135430203, 화합물

시약·촉매·용매 1

HCID 21584188Chloroform methanol용매

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) in tetrahydrofuran (2 mL) was added 1,1′-thiocarbonyldiimidazole (0.042 g). After stirring for 1 hour, silica (1 g) in chloroform:methanol (5:1) (12 mL) was added and the mixture was stirred for a further 12 hours. The solvent was removed under vacuum, the resulting solid was taken up in methanol (20 mL) and was purified by Varian NH2 cartridge (methanol (50 mL) and then acetic acid:methanol 10:90 as eluant) to afford the title product (0.041 g).

후처리

  1. stirringthe mixture was stirred for a further 12 hours
  2. customThe solvent was removed under vacuum
  3. customwas purified by Varian NH2 cartridge (methanol (50 mL)

출처 및 근거

ORD 기록
ord-b0f33582aa884f9f95f81aeb958b915e
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07408065B2

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