Methylamine → Ammonia

HRID 586707ノート

反応式

HRID 586707 の反応式
[CH3:1][NH2:2].[CH2:3]([N:10]1[CH2:19][CH2:18][C:17]2[N:16]=[C:15](Cl)[CH:14]=[CH:13][C:12]=2[CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>CO>[NH3:10].[CH2:3]([N:10]1[CH2:19][CH2:18][C:17]2[N:16]=[C:15]([NH:2][CH3:1])[CH:14]=[CH:13][C:12]=2[CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

5

反応物 2

HCID 6329MethylamineHCID 162287476-Benzyl-2-chloro-5,6,7,8-tetrahydro-1,6-naphthyridine

生成物 2

HCID 222AmmoniaHCID 22335272HCID 22335272、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
140 °C

実験手順

Liquid methylamine (20 mL) was added to a cooled (−70° C.) solution of 6-benzyl-2-chloro-5,6,7,8-tetrahydro[1,6]naphthyridine (WO 9830560) (5.5 g, 21.25 mmol) in methanol (30 mL). The mixture was heated to 140° C. in a sealed vessel for 72 hours, then cooled. The reaction mixture was evaporated under reduced pressure and the residual brown oil purified by column chromatography on silica gel using an elution gradient of dichloromethane:methanol:0.88 ammonia (97:3:0 to 96:4:0.5) to afford the title compound as a white solid, 2.97 g

後処理

  1. temperaturecooled
  2. customThe reaction mixture was evaporated under reduced pressure
  3. customthe residual brown oil purified by column chromatography on silica gel using an elution gradient of dichloromethane

出典と根拠

ORDレコード
ord-142ee26f74054094ba078c2602f8ef70
出典データセット
uspto-grants-2005_08
特許番号
US06936619B2

反応ノート

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