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

HRID 1668835
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HRID 1668835 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
27.5 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8e00028cc6cc4a17b9db62d21a41660a
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989463B2

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