Methylamine → Ammonia

HRID 586707노트

반응식

HRID 586707 반응식
[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

참가 물질

5

반응물 2

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

생성물 2

HCID 222AmmoniaHCID 22335272HCID 22335272, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
140 °C

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-142ee26f74054094ba078c2602f8ef70
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936619B2

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