Ethylenediamine → HCID 68601740, 화합물

HRID 1640518노트

반응식

HRID 1640518 반응식
Cl[C:2]1[CH:3]=[CH:4][N:5]=[C:6]2[C:11]=1[N:10]=[C:9]([O:12][CH3:13])[CH:8]=[CH:7]2.[CH2:14]([NH2:17])[CH2:15][NH2:16]>C(Cl)Cl>[CH3:13][O:12][C:9]1[N:10]=[C:11]2[C:6](=[CH:7][CH:8]=1)[N:5]=[CH:4][CH:3]=[C:2]2[NH:16][CH2:15][CH2:14][NH2:17]

참가 물질

4

반응물 2

HCID 3301EthylenediamineHCID 222443958-Chloro-2-methoxy-1,5-naphthyridine

생성물 1

HCID 68601740HCID 68601740, 화합물수율 51%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
100 °C

실험 절차

A mixture of 8-chloro-2-methoxy-1,5-naphthyridine (1.71 g, 8.81 mmol) and ethylenediamine (1.18 mL, 2 eq.) was heated slowly to 80° C. over 1 h and subsequently up to 100° C. for 2 h. After cooling to rt, the yellow solution was taken in DCM and successively washed with NaHCO3. The aq. layer was back extracted with DCM (3 times) and the combined org. layers were concentrated to afford the title intermediate as a pale yellow oil (0.98 g, 51% yield).

후처리

  1. temperatureAfter cooling to rt
  2. washsuccessively washed with NaHCO3
  3. extractionThe aq. layer was back extracted with DCM (3 times)
  4. concentrationlayers were concentrated

출처 및 근거

ORD 기록
ord-973d97214c57474cac618b88ec5152b3
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08114867B2

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