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Hydroxylamine → 7-(Pyridin-2-yl-quinolin-2-yl-amino)-heptanoic acid hydroxyamide

HRID 404140
ノート
印刷プレビュー

反応式

HRID 404140 の反応式
[OH:1][NH2:2].C([O:5][C:6](=O)[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=1)[C:14]1[CH:23]=[CH:22][C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[N:15]=1)C>CN(C=O)C.CO>[OH:1][NH:2][C:6](=[O:5])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=1)[C:14]1[CH:23]=[CH:22][C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[N:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 787HydroxylamineHCID 585450237-(Pyridin-2-yl-quinolin-2-yl-amino)-heptanoic acid ethyl ester

生成物 1

HCID 468430527-(Pyridin-2-yl-quinolin-2-yl-amino)-heptanoic acid hydroxyamide収率 76%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

HONH2 (50% aqueous, 2 mL) was added to III (90 mg, 0.24 mmol) in DMF (0.5 mL) and MeOH (2 mL) at rt. The reaction mixture was stirred for 48 h, after which the solvents were evaporated under reduced pressure. The resulting residue was dissolved and co-evaporated with toluene (2×10 mL) then was purified by silica gel column chromatography eluting with CH2Cl2/MeOH (100:4) to furnish IV as a colourless oil (66.43 mg, 76%).

後処理

  1. customafter which the solvents were evaporated under reduced pressure
  2. dissolutionThe resulting residue was dissolved
  3. customthen was purified by silica gel column chromatography
  4. washeluting with CH2Cl2/MeOH (100:4)

出典と根拠

ORDレコード
ord-b759f961d010482fafe9cc922fbf89df
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08748458B2

反応ノート

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