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5-Nitrofurfural → 1-(9H-carbazol-4-yloxy)-3-{4-[(5-nitro-2-furyl)methyl]piperazin-1-yl}propan-2-ol

HRID 507336
ノート
印刷プレビュー

反応式

HRID 507336 の反応式
[CH:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[C:4]([O:14][CH2:15][CH:16]([OH:24])[CH2:17][N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[CH:3][CH:2]=1.[N+:25]([C:28]1[O:34][C:31]([CH:32]=O)=[CH:30][CH:29]=1)([O-:27])=[O:26].[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+]>C1COCC1.C(O)(=O)C.ClCCl>[CH:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[C:4]([O:14][CH2:15][CH:16]([OH:24])[CH2:17][N:18]2[CH2:23][CH2:22][N:21]([CH2:32][C:31]3[O:34][C:28]([N+:25]([O-:27])=[O:26])=[CH:29][CH:30]=3)[CH2:20][CH2:19]2)=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 127745-NitrofurfuralHCID 5049666Sodium triacetoxyborohydrideHCID 167304831-(9H-carbazol-4-yloxy)-3-piperazin-1-ylpropan-2-ol

生成物 1

HCID 167307301-(9H-carbazol-4-yloxy)-3-{4-[(5-nitro-2-furyl)methyl]piperazin-1-yl}propan-2-ol収率 29%

試薬・触媒・溶媒 3

HCID 176Acetic Acid触媒
HCID 6344
Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 1-(9H-carbazol-4-yloxy)-3-piperazin-1-yl propan-2-ol (0.5 g 1.54 mmol) in THF (10 mL), was added 2-3 drops of glacial acetic acid, followed by 5-nitrofurfural (0.325 g, 2.3 mmol). To the above solution Na(OAc)3BH (0.98 g, 4.6 mmol) was added carefully at room temperature and the reaction mixture was stirred at room temperature for 6 hours. Subsequently the reaction mixture was diluted with dichloromethane (50 mL), washed with water and brine solution. The organic layer was dried over anhydrous Na2SO4, concentrated, and purified by silica gel column chromatography using dichloromethane/MeOH (9:1) to afford the title compound as a yellow colored solid (0.2 g, 29% yield) with m.p.: 54-59° C. 1H NMR (400 MHz, CDCl3): δ 2.40-2.65 (m, 6H), 2.70-2.80 (m, 4H), 3.67 (s, 2H), 4.20-4.25 (m, 1H), 4.27-4.34 (m, 2H) 6.49 (d, 1H, J=3.6 Hz), 6.67 (d, 1H, J=8.0 Hz), 7.06 (d, 1H, J=8.0 Hz), 7.20-7.50 (m, 5H), 8.27 (s, 1H), and 8.30 (d, 1H, J=8 Hz). MS m/z: 451 (M+1).

後処理

  1. washwashed with water and brine solution
  2. dry with materialThe organic layer was dried over anhydrous Na2SO4
  3. concentrationconcentrated
  4. custompurified by silica gel column chromatography

出典と根拠

ORDレコード
ord-0c6062099b2d4eb18641311a6de49452
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07786142B2

反応ノート

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