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Methyl 1-(4-aminophenyl)cyclopentane-1-carboxylate → HCID 59362913、化合物

HRID 1668815
ノート
印刷プレビュー

反応式

HRID 1668815 の反応式
Cl[C:2]1[C:7]2[CH2:8][CH2:9][CH2:10][C:6]=2[N:5]=[C:4]([CH2:11][CH:12]2[CH2:16][CH2:15][CH2:14][CH2:13]2)[N:3]=1.[CH3:17][O:18][C:19]([C:21]1([C:26]2[CH:31]=[CH:30][C:29]([NH2:32])=[CH:28][CH:27]=2)[CH2:25][CH2:24][CH2:23][CH2:22]1)=[O:20]>C(O)(C)C>[CH3:17][O:18][C:19]([C:21]1([C:26]2[CH:27]=[CH:28][C:29]([NH:32][C:2]3[C:7]4[CH2:8][CH2:9][CH2:10][C:6]=4[N:5]=[C:4]([CH2:11][CH:12]4[CH2:16][CH2:15][CH2:14][CH2:13]4)[N:3]=3)=[CH:30][CH:31]=2)[CH2:22][CH2:23][CH2:24][CH2:25]1)=[O:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 15086389Methyl 1-(4-aminophenyl)cyclopentane-1-carboxylateHCID 59362951HCID 59362951、化合物

生成物 1

HCID 59362913HCID 59362913、化合物収率 63%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 4-chloro-2-cyclopentylmethyl-6,7-dihydro-5H-cyclopentapyrimidine (0.38 g, 1.6 mmol) and 1-(4-amino-phenyl)-cyclopentane carboxylic acid methyl ester (0.35 g, 1.6 mmol) in anhydrous isopropanol (8 mL) was heated at reflux under nitrogen for 8 to 18 hours. Thereafter, volatiles were evaporated under reduced pressure. The residue was triturated with ether and filtered. The solid was dissolved in ethyl acetate, washed with 5% sodium bicarbonate, dried over Na2SO4, filtered, and the filtrate was concentrated under reduced pressure to afford the title compound as a light yellow powder (0.42 g, 63% yield).

後処理

  1. temperaturewas heated
  2. temperatureat reflux under nitrogen for 8 to 18 hours
  3. customThereafter, volatiles were evaporated under reduced pressure
  4. customThe residue was triturated with ether
  5. filtrationfiltered
  6. dissolutionThe solid was dissolved in ethyl acetate
  7. washwashed with 5% sodium bicarbonate
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-63adb21169e146ebb5a0836267e83b45
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07989463B2

反応ノート

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