Tetrahydrofuran → HCID 135430203、化合物

HRID 2217910ノート

反応式

HRID 2217910 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 135430203HCID 135430203、化合物

試薬・触媒・溶媒 1

HCID 21584188Chloroform methanol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) 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).

後処理

  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)

出典と根拠

ORDレコード
ord-b0f33582aa884f9f95f81aeb958b915e
出典データセット
uspto-grants-2008_08
特許番号
US07408065B2

反応ノート

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