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Diisopropylethylamine → benzyl-(2-chloro-6,7-dihydro-5H-cyclopentapyrimidin-4-yl)-ethyl-amine

HRID 1668835
ノート
印刷プレビュー

反応式

HRID 1668835 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]2[CH2:9][CH2:10][CH2:11][C:4]=2[N:3]=1.[CH2:12]([NH:19][CH2:20][CH3:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(N(C(C)C)CC)(C)C>C(O)C>[CH2:12]([N:19]([C:6]1[C:5]2[CH2:9][CH2:10][CH2:11][C:4]=2[N:3]=[C:2]([Cl:1])[N:7]=1)[CH2:20][CH3:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 84352N-EthylbenzylamineHCID 2313312,4-dichloro-5H,6H,7H-cyclopenta(d)pyrimidine

生成物 1

HCID 59362933benzyl-(2-chloro-6,7-dihydro-5H-cyclopentapyrimidin-4-yl)-ethyl-amine収率 99.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
27.5 °C

実験手順

A mixture of 2,4-dichloro-6,7-dihydro-5H-cyclopentapyrimidine (0.4 g, 2.1 mmol), N-benzyl-ethylamine (0.35 mL, 2.3 mmol) and diisopropylethylamine (0.4 mL, 2.1 mmol) in anhydrous ethanol (5 mL) was heated at a temperature in the range of 20° C. to 90° C. for 18 hours. After cooling to about 20 to 35° C., the reaction mixture was concentrated under reduced pressure. The crude residue was diluted with ethyl acetate, washed with water, brine, dried over sodium sulfate, filtered and concentrated under reduced pressure to afford a light pink liquid (0.60 g, 98% yield).

後処理

  1. temperaturewas heated at a temperature in the range of 20° C. to 90° C. for 18 hours
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. additionThe crude residue was diluted with ethyl acetate
  4. washwashed with water, brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-8e00028cc6cc4a17b9db62d21a41660a
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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