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Ethylenediamine → N-[2-(2-Methyl-1,3-dioxolan-2-yl)-4-pyridyl]ethane-1,2-diamine

HRID 333062
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인쇄 미리보기

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HRID 333062 반응식
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2([CH3:13])[O:12][CH2:11][CH2:10][O:9]2)[CH:3]=1.[NH2:14][CH2:15][CH2:16][NH2:17]>>[CH3:13][C:8]1([C:4]2[CH:3]=[C:2]([NH:14][CH2:15][CH2:16][NH2:17])[CH:7]=[CH:6][N:5]=2)[O:12][CH2:11][CH2:10][O:9]1
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참가 물질

3

반응물 2

HCID 3301EthylenediamineHCID 668355144-Chloro-2-(2-methyl-1,3-dioxolan-2-yl)pyridine

생성물 1

HCID 66835538N-[2-(2-Methyl-1,3-dioxolan-2-yl)-4-pyridyl]ethane-1,2-diamine수율 95.2%

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온도
180 °C

실험 절차

4-Chloro-2-(2-methyl-1,3-dioxolan-2-yl)pyridine (500 mg, 2.5 mmol) was mixed with 1,2-diaminoethane (1.09 ml, 26.2 mmol) and stirred in a closed vessel at 180° C. with microwave heating for 30 minutes in two batches. The mixture was evaporated to dryness, the solid residue was washed with acetone. The washing solution was evaporated to dryness and this solid residue was washed with acetonitrile. The solid residues were combined and dried under reduced pressure to yield 531 mg of a solid (2.38 mmol, 95%). MS (APCI) m/z=224.1 [M+H]+.

후처리

  1. temperatureheating for 30 minutes in two batches
  2. customThe mixture was evaporated to dryness
  3. washthe solid residue was washed with acetone
  4. customThe washing solution was evaporated to dryness
  5. washthis solid residue was washed with acetonitrile
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-bec392ac1a5847c486292900401e513b
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08877934B2

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