Triethylamine → HCID 57457809、化合物

HRID 44693

反応式

HRID 44693 の反応式
[NH2:1][CH2:2][C:3]1([OH:8])[CH2:7][CH2:6][CH2:5][CH2:4]1.C(N(CC)CC)C.Cl[C:17]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[N:20]=[CH:19][C:18]=1[N+:27]([O-:29])=[O:28]>ClCCl.O>[N+:27]([C:18]1[CH:19]=[N:20][C:21]2[C:26]([C:17]=1[NH:1][CH2:2][C:3]1([OH:8])[CH2:7][CH2:6][CH2:5][CH2:4]1)=[CH:25][CH:24]=[CH:23][CH:22]=2)([O-:29])=[O:28]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 112758084-Chloro-3-nitroquinolineHCID 130512021-(Aminomethyl)cyclopentan-1-ol

生成物 1

HCID 57457809HCID 57457809、化合物収率 65.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-(aminomethyl)cyclopentanol (approximately 55.2 mmol, prepared as described above) in dichloromethane (280 mL) was added triethylamine (7.76 mL, 55.7 mmol) and 4-chloro-3-nitroquinoline (9.22 g, 44.3 mmol). The mixture was allowed to stand at rt over the weekend. A solid formed that was isolated by filtration. Two more crops of solid were isolated from the mother liquor. The yellow solid was stirred in water and filtered. The solid was washed with water multiple times and was dried under vacuum with heat to give 1-{[(3-nitroquinolin-4-yl)amino]methyl}cyclopentanol as yellow crystals (8.29 g, 52%).

後処理

  1. customto stand at rt over the weekend
  2. customA solid formed that
  3. customwas isolated by filtration
  4. customTwo more crops of solid were isolated from the mother liquor
  5. filtrationfiltered
  6. washThe solid was washed with water multiple times
  7. customwas dried under vacuum
  8. temperaturewith heat

出典と根拠

ORDレコード
ord-277fc0269cae449d89f44ea711dded6a
出典データセット
uspto-grants-2013_09
特許番号
US08541438B2

関連ノート

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