Ethylenediamine → HCID 68601740、化合物

HRID 1640518ノート

反応式

HRID 1640518 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 68601740HCID 68601740、化合物収率 51%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-973d97214c57474cac618b88ec5152b3
出典データセット
uspto-grants-2012_02
特許番号
US08114867B2

反応ノート

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